isolating morphine from pods!

[chemchem]

Ok, well my dry water extract was about 3 grams, which means there should be about one gram of M in there. I should have probably done this on a larger scale but.... I wanted to try

I did the extract with the sodium/calcium carbonate mix, there was some very very fine particulates which I filtered. I then brought the ph down to 9ish and let it sit.. there was some precipitate but I am not sure if it is all M.

I was wondering if anyone knows of a non-water soluble solvent that will dissolve morphine? According to the CRC: insol in H2O, ether, acetone. Soluble in methanol and pyridine, and slightly in ethanol.

Now what I may do is wash this precip with water, that way it will dissolve any of the salts I used before but not the M.

What I really want to do is just a simple extraction with an organic solvent. I believe chloroform also does not dissolve M, but it will do so with codeine.

I'm assuming there is still a lot of other material in this solution, but I must have gotten rid of some with the basification.

[SynthMorph]

Mix it with chloroform and it'll take out all the excess alkaloids and get it really pure. Did you take the solution to ph 12 and filter before going to ph 9?

[robojunkie]

Morphine base is insoluble in virtually every solvent, though moderately so in n-butanol, but this is a bitch. There is no real way to improve the old school isolation prep other than using calcium hydroxide instead of Na2CO3. And if ya wanna really nail it take up the reduced "putty" into ethanol, cool the fuck outta it, and filter off all the gray gunk through diatomaceous earth, evap the alcohol and carry on after dissolving back in water as per the usual method. Once one brings back to pH 9 after the morphinate seperation it really does take 12 to 24 hours for the morphine to precip. It looks like tan dust at the bottom of an amber/brown solution. Usually easier to pour off the mother liquor and rinse/pour than filter unless ya got millipores.

[chemchem]

hm.. i may be in trouble

I use the sod and calc carb to bring it to 12, filtered it and there was some dusty particulate, not a lot though. Then I brought it to ph 9 with ammonium chloride and let it sit in my fridge over night.. there was dusty brown precip on the bottom......

Now if you're saying this dusty brown precip is M then I might be in trouble, to try and get it pure I tried dissolving the M in MeOH since it was one of the only solvents saying it will dissolve and I know the carbonates won't dissolve to well (if that is was I have behind)

Anyways, a lot of the dusty brown precip I got from leaving it in the fridge did not dissolve in the MeOH (hot) and when I evaporated what I got after filtering was a little bit of dusty white powder.

I'm just thinking this dusty powder that didnt dissolve isnt M, it tastes pretty salty and not bitter like I think M would taste, but then again I dont know (I tasted the smallest amount for you safety freaks)

[SynthMorph]

Is it in salt form and if so what salt did you use, hcl? Also you say you only started with 3 g of material that means you could have anywhere from 150mg to 900mg of morphine. Why don't you try a larger amount, makes it more worth your time.

When you filter at ph of 12 and above there should be a lot of alkaloids caught when you filter it, anywhere from 70%-95% of your starting material. I'm assuming you're using CPS.

[chemchem]

No, it is not in salt form. Does just adding concentrated HCl make a good salt? I know last time I was trying to make a M-derivative salt with acetone and hcl, but it didn't work.. came out sort of like silly putty.
I'm trying to keep it in freebase form for further reactions.

I might try the chloroform thing, to give it a wash.

robo: I do have calcium hydroxide, I will try that next time. Why do you say this is an improvement over sod. carbonate? I will also try the ethanol method to try and get it a little cleaner. What I really need is to get some suction filtration going instead of gravity, takes way too long. Also, we call it celite, not as long to type out or say. I'll have to bring some of that and my sinter funnel home. I'm used to crystal formation, not dust.

synth: I am using cps, it was hard to tell how much precipate there was at ph 12 but probably more than what I got from the ph 9. I need a better filtration system.

I plan on doing it on a much larger scale next time, this was just a micro prep to see how it will go. I think if I have enough CPS and better filtration equipment it should work, which will make me super happy because then I won't have to demethylate anything with HBr or PyrHCl.

Does anyone know of a good solvent for recrstallization of M free base? I think EtOH would be good.
I'm going to try and read some more papers to get a better idea of extraction and possible solvents, I want to make sure my stuff is clean.

I got two more questions: How can I test to make sure this brownish powder I have is morphine freebase? Preferably without making it a salt.

I always get this confused, do I want to use qualitative or quantitative filter paper if I want to keep my dusty brown filtrate? I've been using coffee filters because I know they work but I want to do it right (and they don't fit my buchner)

It always amazes me how much difference a methyl group can make with solubility

edit: I read somewhere about adding calcium hydroxide to make the morphenate salt precipitate? I'm assuming you add enough to go to ph9 or does calcium hydroxide just stop dissolving then?

edit2: going back to trying to figure out if I actually have M freebase, does anyone know what it tastes like?

[SynthMorph]

Dilute some hcl and add it to the M base and it'll become morphine hydrochloride. Add some water and add a little bit of chloroform. Swirl it around and let it sit for about 30 min and the chloroform layer will become dirty with all the plant matter and excess alkaloids. Your water layer will contain very pure morphine. Just evaporate and dry in the oven.

[robojunkie]

robo: I do have calcium hydroxide, I will try that next time. Why do you say this is an improvement over sod. carbonate? I will also try the ethanol method to try and get it a little cleaner. What I really need is to get some suction filtration going instead of gravity, takes way too long. Also, we call it celite, not as long to type out or say. I'll have to bring some of that and my sinter funnel home. I'm used to crystal formation, not dust.

synth: I am using cps, it was hard to tell how much precipate there was at ph 12 but probably more than what I got from the ph 9. I need a better filtration system.

I plan on doing it on a much larger scale next time, this was just a micro prep to see how it will go. I think if I have enough CPS and better filtration equipment it should work, which will make me super happy because then I won't have to demethylate anything with HBr or PyrHCl.

Does anyone know of a good solvent for recrstallization of M free base? I think EtOH would be good.
I'm going to try and read some more papers to get a better idea of extraction and possible solvents, I want to make sure my stuff is clean.

I got two more questions: How can I test to make sure this brownish powder I have is morphine freebase? Preferably without making it a salt.

I always get this confused, do I want to use qualitative or quantitative filter paper if I want to keep my dusty brown filtrate? I've been using coffee filters because I know they work but I want to do it right (and they don't fit my buchner)

It always amazes me how much difference a methyl group can make with solubility

edit: I read somewhere about adding calcium hydroxide to make the morphenate salt precipitate? I'm assuming you add enough to go to ph9 or does calcium hydroxide just stop dissolving then?

A procedure, successful I'll add, using pod tea as a starter (about 30 large heads from TPS) yielded in the end somewhere around 300 mg morphine base on the first run. This then yielded about 150 mg or so diamorphine. That's neither here nor there for now, that's the easy part. The hard part is adapting the USP method (calcium hydroxide) to pod tea. Pod tea contains all kinds of excess gums and latex in a much higher prevalence than crude opium. This is why I have found that using the initial ethanol solvation to crash out the gums and gack with a Celite (diatomaceous earth) filtration first then evap/rehydration of the residue (one loses well over half the mass and gets a sticky black tar like real opium) is beneficial. It took industry over a hundred years from Serturner's time to patent a viable morphine extraction from straw.

Anyway the chief benefit of calcium hydroxide is effective alkalinization without concern for too high a pH as Ca(OH)2 is water insoluble. However it will of course be consumed by all the protonated alkaloids and any other base decomposed materials. Carbonate will boil off CO2 leaving sodium hydroxide which can decomp product if too concentrated. The lack of solubility of the slaked lime (the calcium hydroxide) renders pH management unnecessary at the high end.

A simple non-reagent test to at least differentiate the base is this: add a minimum of water, then add (titrate if you have a balance to estimate required volume) white vinegar. If on adding enough you have a light tan solution (I tested this subsequent solution via bioassay, ie I IV'd it, bada bing bada bang!) you almost certainly have morphine base. It really does look like junk, as in crappy plant residues or some shit, but this is a typical phenolic alkaloid (amphoteric), actually typical of most phenols. Phenols are notoriously insoluble in most inorganic and organic solvents. Morphine is a unique material due to its amphoteric nature, (the amine is basic of course and phenols are acidic, not as much as a carboxylic acid moiety, but still acidic) and this is the reason it can be purified simply by acid/base precipiation without even so much as an extraction. If one wants to go balls out on the morphine acetate (easiest salt to make for safer injection, don't fuck with H2SO4 unless you have microsyringes to measure with and a good balance), one can add activated charcoal to the aqueous solution and filter through Celite again, one should get a very lightly tan colored solution then, maybe even colorless. If on acidification it doesn't dissolve, it ain't morphine. Hell, if it "is" and "isn't" ie impure, the acidification should leave behind cellulosic impurities. All the other alkaloids should have come out at the high pH. Of course one could extract the basic filtrate contnaining the calcium morphenate with methylene chloride to try to remove chlorophyls and remaining micro amounts of alkaloids.

As far as filters, dumpthe coffees and use the finest and smoothest filtes like microfine/millipores if you have access and a vacuum. If not I'd pour most of the liquid and tap dry the residue on fine typing paper until dry. One gets quite skilled at this quickly its easier than it sounds.

Phenols are insoluble due to "pi stacking" combined with intermolecular H-bonding. The pi stacking (rings on top of rings) ensures the H-bonding is phenol to phenol and not phenol to water. It isn't really the methyl group its the loss of the phenolic OH. I've posted more extensively, including awrite up on this somewhere in the chem section I believe. From pods to heroin...I vouch for it cause I banged pure diamorphine from it.

[kabouter]

can someone post a recipe for extracting M from poppies?

[Papa Verine]

can someone post a recipe for extracting M from poppies?

There are many threads here on this topic. I did a search one day and read hours of posts on just this topic. In the end I decided to just drink my fuckin tea. I have developed quite the stomach for the stuff. In fact, when I don't drink any tea I piss maybe once a day and it's dark yellow.

[jacky]

I am closing this thread...

should be obvious why, but....

its just that chemchem is discussing this pretty much in an incriminating way.

I am not suggesting that you say "swim did this and that, or my cat is extracting Morphine from pods etc etc"
I know that alot of the swim did this and swim did that threads end up sounding stupid, or threads that focus on a cat performing activitys that even most high school graduates couldnt figure out sound stupid....

but I can be party to letting you guys use this forum as a communication for lab procedure of an activity such as this.

if you want to discuss this....just do so in a way that doesnt incriminate yourself.
if the cops come to my house and sieze my computer, that is it for opiophile you know?
and they will probably find out alot more than we would ever give them credit for as far as names, IP addresses, personal chat room stuff etc etc etc.

just discuss it as a matter of "what if?"
what if this happened,
or
I know a person who did this, why did this happen?

etc etc etc.

I think that people that are doing extractions on pods are taking things into an area that is best left unsaid.
its that type of activity that could get alot of media attention...it could create more of a backlash than someone that is just ordering a product and getting rid of it.
or using as a flower arrangement.

I know just possession of the pod is illegal, discussion of tea, and consumption in the past is ok....
but if discussion of isolation or synthesis work is done...
wrap it in ambiguous statements, or something similiar please.

if it isnt a controlled substance, feel free to discuss any chemistry knowledge or research as you wish.

I know that we have been a little loose in the past, but after closing the pod vendor forum, and trying to get the site into a state that will last, and not cause any problems, we have to be a little more vigilant.

no offence chemchem...

its not the subject as much as the delivery.

thanks and appreciate your posts.

[jacky]

one last request before I re-close this thread.

synack asked me if I could provide this link for the posters to continue the discussion
www.clandestinechemist.com (http://www.clandestinechemist.com/)

I dont mind the content of the post technically....I just mind the self incrimination, gotta protect myself from liabilities like this.

discussing chemistry is fine, just dont link it to a person/place/time.....
thanks guys.

[Synack]

I've setup a new thread for this topic at ClandestineChemist. You can access it here: http://www.clandestinechemist.com/viewtopic.php?f=20&t=21