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Thread: Thought on desomorphine synthesis

  1. #31
    OpioNoMo borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker
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    Default Re: Thought on desomorphine synthesis

    I studied chemistry in collage but that was 25 years+ (I'm OLD) and right after that, I spend 15 years writing computer games (cannot give name, but she hsd bit boobs & raided tombs). Never really used the education.

    I guess the only part I still remember is the techniques for resarching... I've got an external HD just crammed with useful patents/journal articles and so on for all drugs. The cost of the storage space is what kills it. It would be about 25000 PDF files....

    I honestly think that everyone here, if they put in the effort could learn enough to produce totally novel work. Just exploring solvent systems is an immense task.

    The cool thing is, there really is useful, new stuff appearing in patents all the time.

    I know my stuff is REALLY rusty but if anyone asks me a reasonable question, I will always try to answer them. Some more people actually reading papers & finding new technology would make a huge difference. Right now, it seems like it's just me... kind of lonely.

    The other thing is that 2 people working together avoids more errors....

  2. #32
    Occasionally Opiated PcChip is an unknown quantity at this point
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    Default Re: Thought on desomorphine synthesis

    Thanks for your work and your posts; What do you mean "the cost of storage space is what kills it" ? Do you mean physical storage like a room, or electronic storage as in data? If the latter, you can purchase 2 Terabyte hard drives very cheap these days...

  3. #33
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    Default Re: Thought on desomorphine synthesis

    Quote Originally Posted by PcChip View Post
    Thanks for your work and your posts; What do you mean "the cost of storage space is what kills it" ? Do you mean physical storage like a room, or electronic storage as in data? If the latter, you can purchase 2 Terabyte hard drives very cheap these days...
    I would like to post them all on Opiophile, but it's not really practicable.

    As far as the desomorphine synthesis goes, it may be a case in which altering the HI concentration after 6,7 diiodination occurs to prevent loss of the 3-OCH3 (you just want to demethylate, not dehydrate.) I think it will require some serious modelling, but those Russians has great basic theory.

    Once the 6,7 diiodo intermediate is formed, materials such as Zn form an alkene (6,7) in very high yield leaving a product (desoxycodeine-C) that can be deprotected in the usual manner. Hopefully the lower-energy route would prevent the epoxide bridge from being broken (and the phenol from being lost)...

    Just thinking sround the problem but really need tables of pKa and such...
    Last edited by borohydride; 07-06-2011 at 05:33 PM.

  4. #34
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    Default Re: Thought on desomorphine synthesis

    The actual pathway of the codeine->desomorphine synthesis is actually REALLY well thought out. I don't think someone tried it randomly, I think someone worked out the pathway. I also suggest that yield may be drastically improved by a simple modification. The materials listed below are from 'Chromatographic study of expert and biological samples containing desomorphine' JOURNAL OF ANALYTICAL CHEMISTRY Volume 63, Number 4, 361-370 by S. A. Savchuk, S. S. Barsegyan, I. B. Barsegyan and G. M. Kolesov.


    Codeine


    α-iodocodeine


    6,7-diiododihydrocodeine


    Desoxydihydrocodeine


    Desoxydihydromorphine-D (desomorphine).


    The main problem with this route is that to reduce the 2 iodines from the 6,7 dihydrodesocodeine requires the hydroiodic acid to dissociate & this requires a lot of heat. Similar reactions using HBr showed that a significant amount of the molecules has the epoxy bridge broken (22% in concentrated HBr). This leads to such side-products as:


    β-iodomorphide fromed by allylic rearrangement of α-iodocodeine. Hard to reduce.


    Loss of phenolic -OH which requires a lot of energy + very acidic conditions


    Epoxy ring is broken - 1/10 activity

    [img]"http://i55.tinypic.com/24q017t.png"[/img]
    The 1 position is particularly vunerable to attack & radio-labelled 1-iodo derivatives
    are frequently used to track such drugs within thr body. They are supposed to be
    faster acting but do not affect subjective effects.


    HI makes a good iodinating agent both in replacing -OH groups & across alkenes. It seems to me that stopping the process at this stage, reducing the 6,7 di-iodo back to an alkene & then deprotecting the ether in a higher-yielding route would alter things an AWFUL lot. I know that desoxymorphine-C (formed from the reduction of the 6,7 diodo) is just as strong as desomorphine... and legal within the UK.

    I will shortly detail a practical route for making HI using Na2S2O5... not suitable for large amounts needed by meth cooks but sufficient for people turning a few grams of codeine into desoxymorphine!
    Last edited by borohydride; 07-07-2011 at 07:55 AM.

  5. #35
    OpioNoMo borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker
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    Default Re: Thought on desomorphine synthesis

    That last image that I incorrectly posted is thus:






    The 1 position is particularly vunerable to attack & radio-labelled 1-iodo derivatives
    are frequently used to track such drugs within thr body. They are supposed to be
    faster acting but do not affect subjective effects.


    It seems to me that if the reaction could be halted at the 6,7 di-iodo stage, or, if a lower concentration of HI would reduce the 2 groups, then yield would go up. From the patents concerning deprotection using HCl & HBr, a lower concentration of acid combined with a 'rate-accelerant' produced those very high yields. Earlier routes used 48% HBr & yielded around 80% in 20 minutes. 40% HBr with H3BO3 catalyst gave 97.6% yield in 60 minutes.

    If the lower concentration of HI cannot effectively reduce the 6,7 di-iodo then visceral dihalide->alkene is a well known reaction with many variations:

    1-Zn/GAA + Δ
    2-Zn/ethanol + Δ
    3-NaI/acetone
    4-NaOH/ethanol + Δ

    Finding the reaction kinentics so that the appropriate reactions can be calculated is the next step. I suspect that simply running the reaction at a lower temperature will stop at the 6,7 di-iodo step. IF HI (H+, I-) reduction can be employed with lower concentrations of HI (possibly with a Pt catalyst?) then it may be possible to leave it as a 1-pot reaction.

    As for HI, well I suggest that the very much OTC sodium metabisulfite is a good source. Correct me if I'm wrong on this, but:

    Na2S2O5 (sodium metabisulfite) + H2O + I2 ---> 2HI + 2NaHSO3 (sodium bisulfite).
    NaHSO3 (sodium bisulfite) + H2O + I2 ----> 2HI + NaHSO4 (sodium bisulfate).

    The reactions are reversible so usually an acid is added to push the reaction forward BUT as long as the HI is driven off as gas, the reaction is driven forward. Seems ideal for producing the 50-100ml of 57% HI needed for the experimentor in this field....

    Input gratefully recieved!

  6. #36
    OpioNoMo borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker
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    Default Re: Thought on desomorphine synthesis

    Here are some details on the medical form of desomorphine (CAS 427-00-9)

    -Permonid™ (Roche)
    -1ml Ampoules (2mg desomorphine hydrobromide/0.5mg scolopamine/25mg l-ephedrine)

    '...This substance appears to be remarkably active, with an analgesic effect about ten times greater than that of morphine; its toxicity, although likewise exceeding that of morphine, is apparently only three times as great. Its action is described as being very rapid but of short duration, and not accompanied by vomiting. It was developed by Roche and has been given the commercial name of Permonid™ in Switzerland, where it is used...'

    There is only 2 example in the literature concerning a non-accidental overdose of Permonid by a patient in a Swiss hospital. The individual managed to inject 34mg of desomorphine (=340mg of morphine or ≈200mg of diamorphine). Vigerous intervention by staff members succeeded and the patient recovered after about 8 hours. The patient was later moved to a psychiatric ward.
    Last edited by borohydride; 07-08-2011 at 05:05 AM.

  7. #37
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    Default Re: Thought on desomorphine synthesis

    Allyl alcohol + HI ----> allyl iodide (Preparation of allyl iodide J. Am. Chem. Soc., 1948, 70 (8), p 2818 R.L. Letsinger & James G. Traynham.

    Allyl iodide + HI ----> 1,2 diiodopropane (The Mechanism of the Reaction Between Glycerol & Hydroiodic Acid J. Am. Chem. Soc., 1952, 74 (11), pp 2709–2712 R. B. Bradbury.

    The above papers show that codeine + 2HI will form 6,7 diiodo desocodeine:


  8. #38
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    Default Re: Thought on desomorphine synthesis

    I decided to read how the Russians make Krokodil, just to get some insight:

    1. 7 packs Tetralgin (Codeine Phosphate tablets).
    2. 7g iodine.
    3. Gasoline (92 or better 80) half a liter.
    4. Alkaline liquid such as ammonia.
    5. Acetone 0.5l bottle
    6. Barrels 20ml, 10ml
    7. Two bottles of 0.5 and 1.5 of white translucent plastic
    8. Butterfly injection
    9. A couple of vials Pipolfen (injectable antihistamine)
    10. Two/three packaging ordinary matches
    11. Acid HCL 40% (drain cleaner)
    12. bottle of Naphazoline (nasal drops)

    Over all about. 400 rubles with the expectation of three people. All the complexity only because tetralginom for we have only two packets in the snout sell.

    Tetralgin crush to dust and pour into a bottle of 1.5 liter plastikovub.
    Fill a couple of caps of liquid alkali such as "Sleeper" (caps on bases) and shake the bottle until it is covered completely from within the resulting misalignment. After that, fill it with gasoline about 250, and shake for 15 minutes.
    Gasoline akuratno merge into a bottle of 0.5 liter. The main thing that the bottle of gasoline but not horrible or anything. Add 4-5 drops of acid. (The acid can be purchased at auto parts or radios) and shake the bottle for about 5 minutes. Shake to be very strong. Gasoline merge back into the bottle of 1.5, but in our day to remain small white kristaliki codeine. They wash off with acetone in a bowl and wait until all the acetone erode if acetone sucks, then it all fade dick and have it wash away. I do this a syringe 20ml.
    Pour carefully so as not to squander the crystals.


    If necessary, repeat the whole operation once or twice.

    I tend to repeat, because Bottle 1.5 continues to give "gunpowder" (codeine).

    In obtaining crystals of about 5:4 to add red phosphorous. It is usually taken in the laboratory or bought from baryg, but I wash off with normal acetone his matches, then it is still being filtered. Only need to wash! with Cherkashev with 2-3 packs.
    Acetone and then fades or blends, for his speed, I podzhegayu.

    Take our naftezin and pour the contents, we only need a glass stopper with Furyk. His carefully and dry the my. Cork pierced with a pipette or a garage on the accordion with a cutoff tip - called Otto. It will be a reactor.

    The next stage - is iodine. Its all merge into a glass and fill with cold water until it starts to mix with it. This will show red on the surface of the divorce. He settles for about 20 minutes. The water is not completely drained, reserve 8 - 10 ml and select all the contents of the syringe, 10ml. Pushed into the needle and put on cotton wool on the accordion. Water is discharged, and iodine is a bayan. Then we obtain iodine and sushem it between two pages in a thick book. Suffice it once promaknut.Vy can find other ways to get iodine, but the fastest and most economical.

    Iodine fall asleep in our Furyk out of naftezina per OBIN vial per pack tetralgina. I usually fall asleep a little smaller.

    IMPORTANT! - The drier the iodine to react more quickly, I usually just nedosushivayu to reakyiya was a little bit longer, so it's easier to control!

    Add our mixture of red phosphorus and codeine and quickly stoppered c drive away. It is better to immediately roll up with tape, otherwise the reaction can be considered proebanoy. Warm all at the candle until you stop to smoke and shake with Furyk in a circular motion in the horizontal plane. Pour about 8cc of water and boil for 2-3 minutes.
    In the red stone formed Furyk-red color. Choose pure water in 20 ml of an accordion. We took a stone and rubbed it in with water and palovnike boil. Choosing the same accordion. In total, you should have 14cc dissolve. Add 1 cube pipolfen and cool.
    Total 15 cubes for three. According to the first ever better put a cube 3.4. Parish turns out very soft and smooth. If you have to start beating heart in a mad rhythm, then the reaction was squander. Keeps this misalignment hours 2 3.After which can deliver vtorikami. Ie add water in the ladle with mashed stone. Boil again, grind, choose to add a second ampule pipolfen and vmazatsya.


    Not a GREAT translation, but it does show that more effort goes in than most people think.

    -The Codeine is freebased & extracted
    -Codeine salted to extract solid hydrochloride
    -Hydriodic acid made from RP/I
    -Reacted with codeine HCl
    -Mixture warmed (with candle!)
    -Boil off excess liquid


    Can you see what the didn't do? They didn't remove any traces of RP from the system (OK, it's not water soluble, but there will be side-products that are).

    7 Packets of codeine = 8x20x7mg of codeine=1120mg. That makes enough desomorphine (120x codeine) for 3 people. The yield is... just terrible.

  9. #39
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    Default Re: Thought on desomorphine synthesis

    borohydride, I don't see the part where you say they boiled the reaction mixture dry. It doesn't read like that to me.

    Warm all at the candle until you stop to smoke and shake with Furyk in a circular motion in the horizontal plane. Pour about 8cc of water and boil for 2-3 minutes.
    In the red stone formed Furyk-red color. Choose pure water in 20 ml of an accordion. We took a stone and rubbed it in with water and palovnike boil.
    It looks to me like they add the codeine, red phosphorus and iodine to a container, then heat it with a candle until it starts to react, then they mix it around and then add 8 mL of water and boil it for 2-3 minutes. I don't think that you could boil dry 8 mL of water in 2-3 minutes. It really would depend on the container shape, in a watch glass this is probably possible, in a test-tube I don't think it is. And they would be doing this in a test-tube so as to contain the HI fumes so that it would have a chance to react with the codeine.

    After the reaction, they dissolve the reaction mixture with water from a 20 mL syringe along with some "pipolfen".

    So it looks to me like they are shooting up the reaction mixture without adjusting the pH or filtering. Plus I looked up "pipolfen", and found that it is the Russian word for promethazine. Here's some quotes from wikipedia's page on Promethazine:

    In 2009, the U.S. Supreme Court ruled on a product liability case involving promethazine. Diana Levine, a woman suffering from a migraine, was administered Wyeth's Phenergan via IV push. The drug was injected improperly resulting in gangrene and subsequent amputation of her right forearm below the elbow. A state jury awarded her $6 million in punitive damages.
    ...
    On September 9, 2009, the FDA made the decision that a black box warning for injection be put on promethazine stating the contraindication for subcutaneous administration. The preferred administrative route is intramuscular (IM) which reduces risk of surrounding muscle and tissue damage
    So a lot of the gangrene and tissue damage from shooting "Krokodil" is from the promethazine anti-histamine that they add to it, in order to increase the effects.

    Plus if they follow the write up borohydride posted, they are shooting extremely over-acidified reaction mixture without adjusting the pH. That would cause severe tissue damage, and it would leach the calcium out of their bones, as their bodies fight to adjust their blood back to the correct pH range.

    If they would extract the reaction mixture the same way they extracted the codeine from the pills, and then leave out the promethazine, then most likely they wouldn't have all these terrible health effects.

  10. #40
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    Default Re: Thought on desomorphine synthesis

    It seems odd that if they are smart enough to extract codeine powder (OK - with GASOLENE!) then extracting the product (or, rather, mixture of products!) is not carried out. I assumed they boiled to dryness because that much HI wouldn't just be dangerous, it would be bloody excruciating to inject.

    I assume that the epoxy-bridge is the first thing to break down under concentrated HI. Also, the allyl alcohol + HI goes through several steps depending on how much HI there is.

    allyl alcohol ---->allyl iodide ---->diiodo propane---->propene---->2-iodopropane

    A Polish friend who had made/used Krokodil said that what was made was 'not exactly' desomorphine. I cannot work out if he means desoxymorphine-C (6,7 alkene) or methyldesorphine (I don't know how this is formed, but it shows up in all of the street samples!).

    Here are several more, similar routes:

    http://translate.google.com/translat...Fp%3D298%23298

    They are all very basic, they all keep the heat below 60C... interesting...

  11. #41
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    Default Re: Thought on desomorphine synthesis

    BTW - desomorphine Channel http://tor4. ru

    I am just guessing but I think it is the reductive nature of HI that is breaking the epoxy bridge. The normal synthesis of allyl iodide notes that if there is an excess of HI then isopropyl iodide is the main product, otherwise allyl iodide & propene are the main products. With the -OH (and thence I) being secondary, the secondary HI reaction forming isopropyl iodide is less likely to happen. This leaves the unanswered question - will HI + cold codeine ---> desoxycodeine-C ? If so, a much friendlier deprotection would be possible...

  12. #42
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    Default Re: Thought on desomorphine synthesis

    дезоморфина - desomorphine
    йод - iodine
    кодеин - codeine

    I see the main brands used by the DIY 'Krokodil' makers are: Sedan-M, Codelac, Terpincod & Pentalgin. Bet there isn't just codeine in them! I note that Nurofen+ is also making a name for itself in the east.


    I have come across a bit of an issue...


    I read the previous explanation in 'The Mechanism of the Reaction between Glycerol and Hydriodic Acid' by R. B. Bradbury (J. Am. Chem. Soc., 1952, 74 (11), pp 2709–2712). Thus:





    But then this totally disagrees: 'The Action of Hydriodic Acid on Glycerol' by Louis Sattler (J. Am. Chem. Soc., 1932, 54 (2), pp 830–831).

    Vogel's Textbook of Organic Chemistry (3rd Edition)

    Allyl Iodide. Use 29 g. (34 ml.) of allyl alcohol and 340 g. (200 ml.) of 57 per cent, hydriodic acid ; 84 g. of crude iodide are obtained. Upon adding 29 g. (34 ml.) of allyl alcohol to the combined residue in the flask and the aqueous layer and distilling as before, a further 72 g. of crude allyl iodide may be isolated. B.p. 99-101° (mainly 100°). The compound
    is very sensitive to light; the distillation should therefore be conducted in a darkened room and preferably in the presence of a little silver powder.

    A referee on this matter would be greatly appreciated!


    Of course, the vicenal dihalo would be more stable than in the example so IF an addition across the alkene does occur, it's likely to stop at that stage. A basic elimination (via halohydrin?) would then lead to an alkene.
    Last edited by borohydride; 07-11-2011 at 01:22 PM.

  13. #43
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    Default Re: Thought on desomorphine synthesis

    http://www.scribd.com/doc/50981990/B...desoxymorphine <-So HI demethylates dihydrodesoxycodeine just fine but if there is a double-bond in there...

    CONCLUSION - The effects of Krokodil are likely to be mediated by compounds other than desoxymorphine proper. Codeine does not represent a reasonable start material for a single-step synthesis of this material.

    Dihydrocodeine, on the other hand, should work MUCH better, but only experimentation will prove this....

    Off to buy I2, NaHSO3, DHC...

  14. #44
    OpioNoMo borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker
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    Default Re: Thought on desomorphine synthesis

    The only thing to add is that N-Phenethylnordesomorphine is x85 morphine in potency & one would assume (based on the QSAR of the closely related levorphanol analogs) that the 2-thienylethyl & 2-furanylethyl would be even more potent (the latter around x500 M). Of course, the N-phenylethyl is easier/cheaper to produce. Phenylethyl bromide + K2CO3 works FINE.

    N-Demethylation: US Patent 7405301 i)MCPBA/H2O2 ii)FeSO4
    N-Alkylation: US Patent 2885401/US Patent 2970147

  15. #45
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    Default Re: Thought on desomorphine synthesis

    I have JUST enough DHC to give this a try but I'm thinking about the best way to get out all of the actual alkaloid from binders/fillers without losing any. The Russian method (base into non-polar solvent then salt back) looks OK but 500ml of petrol (and PETROL FFS!). I presume the best solvent to use is chloroform (1 gram of codeine monohydrate dissolves in 0.5ml of CHCl3) & failing that, the much easier to obtain trichloroethylene (TCE). The monohydrate is still slightly water soluble but cooling the water right down will help & adding something like NH4Cl will drive it all into the organic layer...

  16. #46
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    Default Re: Thought on desomorphine synthesis

    Quote Originally Posted by borohydride View Post
    I have JUST enough DHC to give this a try but I'm thinking about the best way to get out all of the actual alkaloid from binders/fillers without losing any. The Russian method (base into non-polar solvent then salt back) looks OK but 500ml of petrol (and PETROL FFS!). I presume the best solvent to use is chloroform (1 gram of codeine monohydrate dissolves in 0.5ml of CHCl3) & failing that, the much easier to obtain trichloroethylene (TCE). The monohydrate is still slightly water soluble but cooling the water right down will help & adding something like NH4Cl will drive it all into the organic layer...
    I've only played around with cold water extraction on codeine tablets, I've not done a solvent extraction yet. But I found that filtering the solution through paper filters was impossible due to them blocking almost instantly. So I found that the best way was adding water, then allowing the paracetamol to settle, and then sucking off the water with a pipette. The same thing happened with Peganum harmala seed extract, the ground seeds would block filter papers almost instantly, so adding water, mixing then siphoning off the water from the top of the seed powder, was the best way that I tried for getting around this.

    Now if you want to get maximum yields, then the adding water, mixing then siphoning off the water above the settled powder, will not be an efficient extraction unless you repeat it 10 times or so. So for your DHC extraction, you would be most likely be best off trying some other route.

    Now according to the Merck index entries on druglead.com, one gram of codeine freebase dissolves in:
    One gram dissolves in 120 ml water, 60 ml water at 80°, 2 ml alcohol, 1.2 ml hot alcohol, 13 ml benzene, 18 ml ether, 0.5 ml chloroform; freely sol in amyl alcohol, methanol, dil acids. Almost insol in petr ether or in solns of alkali hydroxides.
    Unfortunately it's entry on dihydrocodeine doesn't give any solubility data for DHC freebase, but it should be similar to codeine's solubility.

    Because of the filter blocking issue with codeine tablets in water, using a solvent to extract may well be much better. I have heard of people adding sodium carbonate solution to powdered codeine tablets, mixing to a wet paste (this freebases the codeine) then drying it in the oven. Once dry, they extracted the pill mass with solvent. I can't remember what they used, but it may be worth a try.

    Now because codeine freebase is so soluble in alcohol, that would be my first choice, because toxic solvent fumes are not going to be a problem, and ethanol is a thin solvent, that runs through filters very easily. I would avoid using isopropyl alcohol, because it is so thick, that it makes filtering a pain. And methanol fumes are poisonous, so I'd avoid using methanol as well.

    Now paracetamol is much more soluble in ethanol than it is in water, so as well as extracting the codeine into ethanol, quite a bit of paracetamol will also dissolve in the ethanol. However it may be worth it to get all of the DHC extracted from the bulk of the pill mass. I don't know for sure, because I've never done it. So it's a case of trying one pill at a time in a test tube, until you find a solvent that extracts the DHC but leaves >50% of the pill mass undissolved, and where the solvent is filterable away from the pill mass.

    So if ethanol doesn't dissolve all of the paracetamol, and is filterable, then I would like to use that. Because 1 gram of codeine dissolves in 2 mL of ethanol, then if you distil down the ethanol to a small amount, say 50 mL and you see crystallisation but there is only 1 gram of DHC in the ethanol solution, then you'd know most likely that what was crystallising out wasn't the DHC, and was probably the paracetamol. That may work, it may not, only experimentation will let you find out for sure.

    Finally the Merck entry on acetaminophen (paracetamol) says that it is practically insoluble in petr ether, pentane, benzene. Don't use benzene because it's causes cancer, but benzene and toluene are similar and dissolve similar things, and as one gram of codeine dissolves in 13 mL of benzene, it should take a similar amount of toluene.

    So once you have a small pile of extracted DHC freebase, you should be able to separate it from any paracetamol, by extracting it with toluene, I'd try extracting the powder 3x with 15 mL toluene per gram of DHC freebase. The DHC should dissolve, while the paracetamol wouldn't dissolve, and could then get filtered out. The toluene could then either get dried and gassed with HCl to recover DHC hydrochloride, or evaporated off to leave you with DHC freebase.

    DHC is crystallised from methanol + water, so a dual solvent crystallisation with ethanol and water should also work. Dissolve the DHC in a few mL of ethanol then add hot water until it starts to crash out, then add drops of ethanol until it redissolves in the hot water / ethanol mix, and then cover it and allow it to slowly cool.

    It's kind of a pain with extractions until you find what works, so just stick to using a pill at a time until you find a method that works and is filterable. Ethanol would be no good of it dissolved all the paracetamol, but if you add 10 mL ethanol to 1 gram of powdered pre-basified pill mass and it only dissolves 50% the powder or less, then it would be worth it to help remove the DHC freebase from the pill binders and stuff.

    Chloroform, dichloromethane and trichloromethane all dissolve similar things, but dichloromethane is probably the easiest and cheapest to get, as it's the main chemical in paint remover, and because of it's low boiling point, it's easy to distil it out of the cans. I heard of people sticking a bung with a still head directly into the paint can, and distilling it directly from the can by sticking the can in a hot water bath.

    Basing the pill mass with sodium carbonate solution then drying, is most likely going to be the first thing necessary, as codeine hydrochloride and codeine sulphate are not very ethanol soluble. So you'll have to do that whether you extract with ethanol first or toluene or dichloromethane. But I would advise against trying to extract the pill mass with non-polar solvent, because it will take a huge volume of solvent, the solvent is expensive, and the fumes are really bad for your health.

    As I've not done it, I don't know which solvent extraction of pills works. But because the alkaloids are so insoluble in high pH water, you may find through experimentation that manipulating the pH of water works well enough. However if you basify the water, then instead of trying to extract the precipitated DHC from the water with solvent, it's better to filter them out, then extract the water with solvent to remove the rest. But you may find like I did, that pill binders make filtering the cold water extract impossible due to blocking up the filter paper.

    In that case, if you really want to extract the high pH water with solvent, then I'd recommend trying dichloromethane first, because it sinks, so as the precipitate drops, it will come in contact with the solvent, and dissolve into it. I have found that when mixing toluene with precipitated DMT, it didn't work well, because the DMT sunk to the bottom of the flask and the toluene floated above the water, so they didn't mix well.

    That's it really, good luck with your experimentation, I hope it works well for you.

  17. #47
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    Default Re: Thought on desomorphine synthesis

    ^^ Haven't read the entire post, yet, but the trick to filtering is to pre-wet the filter medium with water. Doing this allows you to use anything from coffee filters to toilet paper to gas station napkins as the filter medium..
    All posts made under the user account 'Chopstix' are exercises of creative fiction and in no way represent fact or truth. The user account 'Chopstix' is open to multiple authors with a common interest in lawful research and authoring fiction; and as such, no single user is responsible for the entirety of the post content of this account. No content may be reproduced in any form or fashion via any medium whatsoever unless specified with written and notarized permission of the original post author, without exception. Got that? Good! Have a bitchin' day.

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  18. #48
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    Default Re: Thought on desomorphine synthesis

    Gentlemen-

    It is actually easier to to from 8-bromomorphide and Hydrogenate in a beer bottle (or a garden sprayer with a pressurized pump) with a balloon (H2 gas in balloon) and pd/c as the catalyst.

    To get to 8-bromomorphide all you need is 15% HBr in acetic acid, reflux codeine in it for a few hours.

    Easy peasy.......

    I'll let you peeps know what I figure out.
    "he scores......... he shoots!!!!"
    - Kirkinov

  19. #49
    OpioNoMo borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker
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    Default Re: Thought on desomorphine synthesis

    You refer to 'Practical and High-Yield Syntheses of Dihydromorphine from Tetrahydrothebaine and Efficient Syntheses of (8S)-8-Bromomorphide' which I posted on this site last year.

    Now, since your the expert, point to a paper where they SUCCESSFULLY performed your 'beer bottle' hydrogenation?

  20. #50
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    Default Re: Thought on desomorphine synthesis

    I really don't want to post all the info I have on the open board as I'm not really
    trying to get anyone to try this as I have yet to do it myself.

    And yes, a beer bottle is a poor hydrogenation vessel, a garden sprayer is much better. Hell, a Parr reactor is the true way to go but lets be honest. I don't have that type of $$ around.

    I tried to discuss this with you off the board, and you ignored me for some reason and now you want to call me out?!?!!

    I don't understand- Is it just the fact that I tried to speak with you privately? or do you just believe when it comes to discussion of synths it needs to be out in the open?

    And.......yes, there's a lot more than what I said to it. I purposely left out parts. If someone wants to make it they can either search for the answers or figure them out. All the info is out there, it just needs to be put together.

    I brought the info to you and you seemed uninterested. So I kept it to myself.

    read this well type in dihydrodesoxymorphine and you'll see some answers.

    And while we're at it, I've noticed many of your summaries are well, not quite right. You, for example use DHC----> DHM and say simply throwing in brick cleaner (HCl) and borax (Na2B4O7) and reflux for 26 hours will make DHM.

    Not quite right, hell that's actually not even close. Not to mention if you just use simple codeine in this process you'll end up puking your guts out since the double bond needs to be reduced before you can hit codeine based molecules with HBr. Otherwise the ether linkage will be broken and apomorphine/apocodeine will be made. Good luck with that shit.
    "he scores......... he shoots!!!!"
    - Kirkinov

  21. #51
    Never Looked Back Spork is a name known to all Spork is a name known to all Spork is a name known to all Spork is a name known to all Spork is a name known to all Spork is a name known to all Spork is a name known to all Spork is a name known to all Spork is a name known to all Spork is a name known to all Spork is a name known to all Spork's Avatar
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    Default Re: Thought on desomorphine synthesis

    Mmmm I love me a good shot of green disgusting apomorphine...
    Spork. Not a Sp(F)o(rk)on

  22. #52
    OpioNoMo borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker
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    Default Re: Thought on desomorphine synthesis

    Quote Originally Posted by dizzle View Post
    And while we're at it, I've noticed many of your summaries are well, not quite right. You, for example use DHC----> DHM and say simply throwing in brick cleaner (HCl) and borax (Na2B4O7) and reflux for 26 hours will make DHM.

    Not quite right, hell that's actually not even close. Not to mention if you just use simple codeine in this process you'll end up puking your guts out since the double bond needs to be reduced before you can hit codeine based molecules with HBr. Otherwise the ether linkage will be broken and apomorphine/apocodeine will be made. Good luck with that shit.
    Codeine is not DHC - no allyl rearrangement, no problem. That is WHY I specified DHC.

    OK - SHOW me the book. I spent a week reading every single attempt at hydrogenation of 8-halomorphides & guess what? They all failed.

    Your ignorance, arrogance & laziness are 3 pretty good reasons why I didn't bother helping you to your super-legal opioid to get rich off.

    Now, actually give a reference or admit your a damned idiot. If you can, then I will be happy to admit that I'm the idiot - but only IF.

    PS Why don't you actually READ about an apomorphine transformation? Some oft repeated myth from the net doesn't match up to the conditions needed to cause such a rearrangement. If your over enthusiastic with codeine, you just get pseudomorphine (allomorphine).

    --- auto merge ---

    BTW folks, if anyone wants to read our 'secret E-mails' then I can easily hand out my invented account & password - I've got nothing to hide....

  23. #53
    your nizzle dizzle is cooler than ice dizzle is cooler than ice dizzle is cooler than ice dizzle is cooler than ice dizzle is cooler than ice dizzle is cooler than ice dizzle is cooler than ice dizzle is cooler than ice dizzle is cooler than ice dizzle is cooler than ice dizzle is cooler than ice dizzle's Avatar
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    Default Re: Thought on desomorphine synthesis

    my arrogance? really? where the hell was I arrogant?

    Dude, I have it right here..........

    National Research Council (U.S.). Committee on drug addiction
    National Academies, 1941 - Psychology - 1581 pages

    And read page 381-382


    Hydrogenation of Bromomorphide.—Bromomorphide was prepared by the method of Schryver and Lees" and purified from methanol. It sintered and darkened at 184°, and melted above 200°. In methanol it showed [a111 +73.9° (c a 2.788). When bromomorphide was hydrogenated in methanol, with Pd-BaSO4, 4.85 g. of alkaloid took up 1.86 moles of hydrogen, and yielded 1.0 g. of dihydrodesoxymorphine-D hemi¬hydrate. The remaining material was a viscous oil, containing a trace of the high-melt¬ing base mentioned under a-chloromorphide. The oil did not give a crystalline ether on treatment with diazomethane. The methylation product in benzene with methyl iodide gave a methiodide of m. p. 235-238°, which appeared to be amorphous, and could be purified only by washing with acetone. It was not the monomethiodide of a dimolecular base, for analysis showed 29.51% iodine, and its properties were not those of bis-dihydrodesoxycodeine dimethiodide. The hydrogenation of bromomor¬phide in methanol with platinum oxide gave onlra small amount of crystalline product, which proved to be tetrahydrodesoxymorphine.
    Hydrogenation of bromomorphide in dilute hydrochloric acid gives more crystalline material than in methanol. From 4.85 g. of bromomorphide, absorption of 1.87 moles of hydrogen, 2.4 g. of dihydrodesoxymorphine-D hemihydrate, 0.2 g. of tetrahydrodesoxy¬morphine, and 1.2 g. of uncrystallizable oil were obtained.


    Is what it says...........now there's no need to be a fuckin dick. We're all on the same side here and for that matter we're all just talking (typing)

    And really I don't need your help, I asked you things because I respect your opinion.

    If you don't want to reply, fine. I left you alone, didn't I? Damn man, there ain't no reason for that shit.
    Now can we leave it behind us? or are we going to become internet enemies? and everytime one of us posts the other is going to follow and spend half their day proving them wrong.

    And when the day is done and you've proved me wrong or vice versa, what the fuck does it really matter?

    I've never said a negative thing about you and personally still respect you, although you didn't have to do me like that...... Ignore me, then put me on blast in the thread.

    So can we leave this shit??
    "he scores......... he shoots!!!!"
    - Kirkinov

  24. #54
    OpioNoMo borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker
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    Default Re: Thought on desomorphine synthesis

    Funny if it wasn't so sad. The started from alpha-bromomorphide (the Br in place of the 6-OH), not beta-bromomorphide (Br at 8), as produced by the HBr/AA method.

    Science is in the details, my friend ;-)

    That epoxy bridge makes the 6 more labile...

    But, good that your reading stuff, I have to give you that.

    Just get noroxymorphone from china & perform a Leuckart-Wallach with phenylacetaldehyde. Job done...

    US Patent application 2010/0210843/A1 (Aug 19) is the reference. 90%+ yield of a product about x80M should buy that Ferrari ;-)
    Last edited by borohydride; 09-09-2011 at 04:14 PM. Reason: Chill man - sorry I got heated back there...

  25. #55
    your nizzle dizzle is cooler than ice dizzle is cooler than ice dizzle is cooler than ice dizzle is cooler than ice dizzle is cooler than ice dizzle is cooler than ice dizzle is cooler than ice dizzle is cooler than ice dizzle is cooler than ice dizzle is cooler than ice dizzle is cooler than ice dizzle's Avatar
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    Default Re: Thought on desomorphine synthesis

    I thought when they said it was prepared by the schryver and lees that implied it was 8 bromo, not alpha bromo.
    they are talking about alpha chloromorphide, but never say alpha bromo, they say bromo prepared by schryver and lees which I thought was 8 bromo.

    Well, whatever, I don't really want to get into it anymore, I just thought it was a simple route that would help this discussion. No, I clearly don't have a Ph.D in chem. I went to college for chem but didn't give a fuck about organic at the time and paid very little attention to medicinal chem, so I am very likely wrong, but I'm trying here man.

    And no I'm not lazy. I read most all the references you post and then reread them and reread again to try to grasp WTF is happening.
    "he scores......... he shoots!!!!"
    - Kirkinov

  26. #56
    OpioNoMo borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker
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    Default Re: Thought on desomorphine synthesis

    I've been blown up with the best ;-)

    dizzle - sorry I was harsh. That last ref I gave you is really your best bet, BE CAREFUL!!!

  27. #57
    your nizzle dizzle is cooler than ice dizzle is cooler than ice dizzle is cooler than ice dizzle is cooler than ice dizzle is cooler than ice dizzle is cooler than ice dizzle is cooler than ice dizzle is cooler than ice dizzle is cooler than ice dizzle is cooler than ice dizzle is cooler than ice dizzle's Avatar
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    Default Re: Thought on desomorphine synthesis

    Did you seriously blow up your lab??????

    How the hell did you do that?

    Care to share?
    "he scores......... he shoots!!!!"
    - Kirkinov

  28. #58
    OpioNoMo borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker borohydride is one bad motherfucker
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    Default Re: Thought on desomorphine synthesis

    Not really; suffice to say we made the top headline of the national news in the country where it happened...

    Tip - when the synthesis specifies a H2O quench, don't use IPA and THEN H2O. 25l of toluene from RT to BP in about 10 seconds... not a nice memory. We got lucky, but my mistake could have cost the lives of two people I love dearly (friends, not family).

    I tell you this because I don't want to see YOU in the news. A few reports on 'new designer terror' might be good for my morale. Oh, and a nice anonymous picture of the wheels/house/boat/business.... life you get. My fingers (and toes) are crossed for you, man!

    --- auto merge ---

    Of, if you suffer asiaphobia - a US answer:




    Synthesis of noroxymorphone hydrochloride
    -----------------------------------------

    Noroxymorphone has previously been synthesized from other opiates, such as morphine (1),
    codeine (2), or thebaine (3) in good overall yields. However, several synthetic steps are required and, as previously stated by Iijima et al. (4), noroxymorphone is difficult to purify. Although noroxymorphone is used in the manufacturing of naloxone, it is not commercially readily available for research purposes. Naloxone, however, is readily available and differs from noroxymorphone only by having an allyl group in the nitrogen. We reasoned that direct N-deallylation of naloxone would provide an easy access to a small-scale synthesis of pure noroxymorphone for research purposes.

    A practical method for the N-deallylation of naloxone hydrochloride to afford noroxymorphone hydrochloride is presented. The N-deallylation was accomplished by rhodium-catalyzed (Wilkinson’s catalyst) isomerization of N-allyl to enamine, followed by hydrolysis of the enamine under the reaction conditions. The catalyst is not soluble in water under normal conditions and therefore such deallylations are typically done in a mixture of water and an organic solvent such as acetonitrile. However, the catalyst seems to be soluble in water, to some extent, at very high temperatures because when a heterogeneous mixture of naloxone in water and 5 to 10 mole percent of the catalyst was stirred at 200 °C for 30-60 min, a complete N-deallylation was observed (as determined by the complete disappearance of the olefinic protons between 5.50 and 6.00 ppm in the 1H NMR spectrum). When the reaction was performed at 150 °C or without the catalyst, no N-deallylation was observed at all. The developed microwave-assisted and rhodium-catalyzed N-deallylation method for preparing noroxymorphone is facile and robust. See also WO/2008/096046.




    Experimental
    Naloxone hydrochloride dihydrate (56 mg, 0.14 mmol (MW=399.87)) was dissolved in ion-exchanged water (2 mL) in a microwave reactor vial. Wilkinson’s catalyst (RhCl(PPh3)3) (10 mol-% ∴ 23.2% by weight ∴ 13mg) (MW = 925.22) was added and the vial was sealed. Argon was bubbled through the heterogeneous mixture for 30 min to remove any dissolved oxygen. The mixture was heated to 200 °C for 60 min, cooled to room temperature and filtered through C18 column to remove the catalyst and a small amount of triphenylphosphine oxide formed in the reaction. The column was further eluted with water (10 mL). The water was evaporated in vacuo to afford pure noroxymorphone hydrochloride in quantitative yield. The structural and analytical data are in accordance with those previously published (1). 1H and 13C NMR spectra of the product are shown in Figures 1a and 1b, respectively.
    NOTES
    Microwave heating is not vital, but desirable. A tinyclave/hydrothermal type pressure vessel with oil bath or similar heating method will work, allbeit more slowly. Chinese manufacturers supply this type of vessel (with Teflon inner lining) for around $220/25 ml (KH25).

  29. #59
    Never Looked Back Spork is a name known to all Spork is a name known to all Spork is a name known to all Spork is a name known to all Spork is a name known to all Spork is a name known to all Spork is a name known to all Spork is a name known to all Spork is a name known to all Spork is a name known to all Spork is a name known to all Spork's Avatar
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    Default Re: Thought on desomorphine synthesis

    I wonder what the most potent opioid ever would be. There must be a ceiling as far as potency by weight goes. I wonder what it might be.
    Spork. Not a Sp(F)o(rk)on

  30. #60
    True Opiophile upstate_007 is one bad motherfucker upstate_007 is one bad motherfucker upstate_007 is one bad motherfucker upstate_007 is one bad motherfucker upstate_007 is one bad motherfucker upstate_007 is one bad motherfucker upstate_007 is one bad motherfucker upstate_007 is one bad motherfucker upstate_007 is one bad motherfucker upstate_007 is one bad motherfucker upstate_007 is one bad motherfucker upstate_007's Avatar
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    Default Re: Thought on desomorphine synthesis

    I think we need a sort of opiophile matchmaking service. Pairing chemists with wealthy benefactors or investors.

    I get 10% of the resulting product for coming up with the idea.
    it's up or out and the ladder's on fire

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