jay
02-16-2005, 06:04 AM
I found this on the net on a codeine information site,any comments?and iam still looking for a way to get rid of the caffiene from the CWE extraction.Appreciate your help.
Having tried the cold water method and finding the yield intolerable, I set out to find a better way of extracting codeine (http://codeine.50g.com/info/codeine.html) from your basic T3's. I think I've hit on a better method with a lot better yield (>90%)
To do this, you will need some chloroform or other solvent in which codeine (http://codeine.50g.com/info/codeine.html) base will dissolve, APAP won't. Merck says that chloroform works best, although I suspect that methylene chloride will work just as well. Ether will work, but it's just too dangerous for my taste. You will also need some dry sodium carbonate. (bicarb might work here, although I haven't tried it.) DO NOT USE SODIUM HYDROXIDE, IT REACTS WITH THE APAP TO FORM SOME SORT OF EVIL LOOKING BLUE GOOP. Na(CO3)2 WILL RAISE THE pH JUST FINE. Lastly, you will need a large pyrex lasagna pan in which to evaporate your product to dryness.
First, place uncrushed T3's or other APAP/codeine (http://codeine.50g.com/info/codeine.html) product in a small glass or beaker and cover with enough distilled water so that the pills will break down into a thin paste. For 30 T3's, I use about 30-35 ml of H20. Let the pills soak until completely broken down into paste. Next add about 5-8 grams of dry sodium carbonate to reduce the codeine phosphate to codeine (http://codeine.50g.com/info/codeine.html) base. The paste will thicken somewhat and bubbles of CO2 will form in the paste as the codeine phosphate is reduced. Add enough distilled water so that the mixture is about the consistency of thin pancake batter and stir the mixture thoroughly with a wooden or glass rod. The pH of the mixture should be about 11 or greater. If it isn't, add more Na(CO3)2 until it is.
Next, pour the mixture into the pyrex pan and rinse the beaker with a few ml of distilled water and add the rinse water to the mix in the pan. Use the stir rod to spread the grayish mixture around the pan so that the layer is as thin as possible. Let the mix dry overnight. You can pop the pan into an oven set to warm, (no hotter), if you want to speed things up.
After the mixture has completely dried, use a single-edge razor blade to scrape the mixture from the pan. It should just flake off in slabs. Now, wrap the dried material in a coffee filter and crush it so that the pieces are about the size of grains of rice. It isn't necessary to grind the stuff any finer, since it would probably clog the filter in the last step anyhow. Pour the dry crushed mixture into a glass bottle with a screw-on top and pour in enough chloroform to completely cover the "gravel" in the bottle. Seal the bottle and shake for a few minutes. Let the contents settle for a minute or two while you set up a gravity filtering apparatus. This can be a coffee filter in a metal strainer, or if you have it, a piece of filter paper in a glass filter funnel. You can't use plastic because the chloroform will attack it and ruin your product. Clean and dry the pyrex pan and set it under the filter to catch the filtered chloroform. Shake the chloroform/"gravel" mixture and pour it into the filter, letting the chloroform/codeine (http://codeine.50g.com/info/codeine.html) mixture run into the glass pan. Let the chloroform evaporate while you put the wet gravel back into the bottle and shake with a fresh portion of chloroform. It isn't necessary to use as much as you did the first time. Again pour the chloroform/gravel mix into the filter paper.
After the second portion of chloroform has run through the filter, you can drip a few ml of clean chloroform onto the filter paper and wet gravel to get the last bit of codeine (http://codeine.50g.com/info/codeine.html) from the APAP and chalk. You should set the glass pan with the chloroform outside to evaporate to dryness. Do not place it into an oven to force dry it. While chloroform is not very flamable, I found out the hard way that chloroform vapor is broken down on contact with the heating elements of the stove to form deadly phosgene gas.
Be patient, soon enough you will have nearly pure codeine (http://codeine.50g.com/info/codeine.html) base in the bottom of the glass pan. After the codeine (http://codeine.50g.com/info/codeine.html) has evaporated, you might notice that the codeine (http://codeine.50g.com/info/codeine.html) is sticky. This is because evaporating chloroform gets very cold and room humidity will condense into the mixture. If this happens, you can oven warm the codeine (http://codeine.50g.com/info/codeine.html), but only after you can no longer smell the chloroform in it. You can now use the razor blade to scrape up the crude product. The codeine (http://codeine.50g.com/info/codeine.html) base will not weigh as much as an equivalent amount of codeine phosphate, because you have stripped the phosphate ions and left behind the pure alkaloid. Fear not, it is still potent orally, just remember to adjust your dose downward. codeine (http://codeine.50g.com/info/codeine.html) base weighs only 75.3% as much as an equimolar amount of codeine phosphate. If you want to re-salt it, you can use the following proces:
Into 20 ml of acetone add 2 ml of phosphoric acid and set this mixture aside. Dissolve your crude codeine (http://codeine.50g.com/info/codeine.html) base into enough acetone so that it just dissolves. You might have to warm up the acetone to get it to dissolve completely. If you want to clean up any insoluble contaminants at this point, take a pasteur pipet and pack a small wad of cotton into the point where the pipet narrows. Using another pipet, drip the codeine (http://codeine.50g.com/info/codeine.html)/acetone mixture through the cotton. Follow this with a ml or two of clean acetone to get all the codeine (http://codeine.50g.com/info/codeine.html) from the pipet filter. Next, mix the acetone/phosphoric acid solution into the acetone/codeine (http://codeine.50g.com/info/codeine.html) base solution in a 50/50 ratio. As you stir the resultant misture, you will see the codeine phosphate quickly precipitate from the acetone as a sticky gummy mass. As you stir the solution, the final product should form a bolus on the stirring rod and look like a wad of chewing gum. Rinse the bolus in a small amount of fresh acetone and then smear it on a glass plate to dry. As the acetone evaporates, the codeine phosphate (CP) will appear to melt. This is because the CP is highly hygroscopic and is absorbing water from the air. Gently warm the CP in an oven to drive off the last of the acetone and then use a pipet or syringe to first drip water onto the CP, and then suck up the CP solution. You may now drink your product, or you can again reduce it to codeine (http://codeine.50g.com/info/codeine.html) base and extract it with chloroform if you prefer a much purer, powdered product.
Even after two acid-base extractions, I have gotten up to 93% of the available codeine (http://codeine.50g.com/info/codeine.html) from T3's with absolutely zero APAP in the finished product. If you choose codeine (http://codeine.50g.com/info/codeine.html) base as your final product, you can now easily turn it into even yummier alkaloids, but that is for another posting.
Sorry about the long cross-posting, but I believe in sharing information which will result in a purer (read: safer) final product. B.B. Welch
Having tried the cold water method and finding the yield intolerable, I set out to find a better way of extracting codeine (http://codeine.50g.com/info/codeine.html) from your basic T3's. I think I've hit on a better method with a lot better yield (>90%)
To do this, you will need some chloroform or other solvent in which codeine (http://codeine.50g.com/info/codeine.html) base will dissolve, APAP won't. Merck says that chloroform works best, although I suspect that methylene chloride will work just as well. Ether will work, but it's just too dangerous for my taste. You will also need some dry sodium carbonate. (bicarb might work here, although I haven't tried it.) DO NOT USE SODIUM HYDROXIDE, IT REACTS WITH THE APAP TO FORM SOME SORT OF EVIL LOOKING BLUE GOOP. Na(CO3)2 WILL RAISE THE pH JUST FINE. Lastly, you will need a large pyrex lasagna pan in which to evaporate your product to dryness.
First, place uncrushed T3's or other APAP/codeine (http://codeine.50g.com/info/codeine.html) product in a small glass or beaker and cover with enough distilled water so that the pills will break down into a thin paste. For 30 T3's, I use about 30-35 ml of H20. Let the pills soak until completely broken down into paste. Next add about 5-8 grams of dry sodium carbonate to reduce the codeine phosphate to codeine (http://codeine.50g.com/info/codeine.html) base. The paste will thicken somewhat and bubbles of CO2 will form in the paste as the codeine phosphate is reduced. Add enough distilled water so that the mixture is about the consistency of thin pancake batter and stir the mixture thoroughly with a wooden or glass rod. The pH of the mixture should be about 11 or greater. If it isn't, add more Na(CO3)2 until it is.
Next, pour the mixture into the pyrex pan and rinse the beaker with a few ml of distilled water and add the rinse water to the mix in the pan. Use the stir rod to spread the grayish mixture around the pan so that the layer is as thin as possible. Let the mix dry overnight. You can pop the pan into an oven set to warm, (no hotter), if you want to speed things up.
After the mixture has completely dried, use a single-edge razor blade to scrape the mixture from the pan. It should just flake off in slabs. Now, wrap the dried material in a coffee filter and crush it so that the pieces are about the size of grains of rice. It isn't necessary to grind the stuff any finer, since it would probably clog the filter in the last step anyhow. Pour the dry crushed mixture into a glass bottle with a screw-on top and pour in enough chloroform to completely cover the "gravel" in the bottle. Seal the bottle and shake for a few minutes. Let the contents settle for a minute or two while you set up a gravity filtering apparatus. This can be a coffee filter in a metal strainer, or if you have it, a piece of filter paper in a glass filter funnel. You can't use plastic because the chloroform will attack it and ruin your product. Clean and dry the pyrex pan and set it under the filter to catch the filtered chloroform. Shake the chloroform/"gravel" mixture and pour it into the filter, letting the chloroform/codeine (http://codeine.50g.com/info/codeine.html) mixture run into the glass pan. Let the chloroform evaporate while you put the wet gravel back into the bottle and shake with a fresh portion of chloroform. It isn't necessary to use as much as you did the first time. Again pour the chloroform/gravel mix into the filter paper.
After the second portion of chloroform has run through the filter, you can drip a few ml of clean chloroform onto the filter paper and wet gravel to get the last bit of codeine (http://codeine.50g.com/info/codeine.html) from the APAP and chalk. You should set the glass pan with the chloroform outside to evaporate to dryness. Do not place it into an oven to force dry it. While chloroform is not very flamable, I found out the hard way that chloroform vapor is broken down on contact with the heating elements of the stove to form deadly phosgene gas.
Be patient, soon enough you will have nearly pure codeine (http://codeine.50g.com/info/codeine.html) base in the bottom of the glass pan. After the codeine (http://codeine.50g.com/info/codeine.html) has evaporated, you might notice that the codeine (http://codeine.50g.com/info/codeine.html) is sticky. This is because evaporating chloroform gets very cold and room humidity will condense into the mixture. If this happens, you can oven warm the codeine (http://codeine.50g.com/info/codeine.html), but only after you can no longer smell the chloroform in it. You can now use the razor blade to scrape up the crude product. The codeine (http://codeine.50g.com/info/codeine.html) base will not weigh as much as an equivalent amount of codeine phosphate, because you have stripped the phosphate ions and left behind the pure alkaloid. Fear not, it is still potent orally, just remember to adjust your dose downward. codeine (http://codeine.50g.com/info/codeine.html) base weighs only 75.3% as much as an equimolar amount of codeine phosphate. If you want to re-salt it, you can use the following proces:
Into 20 ml of acetone add 2 ml of phosphoric acid and set this mixture aside. Dissolve your crude codeine (http://codeine.50g.com/info/codeine.html) base into enough acetone so that it just dissolves. You might have to warm up the acetone to get it to dissolve completely. If you want to clean up any insoluble contaminants at this point, take a pasteur pipet and pack a small wad of cotton into the point where the pipet narrows. Using another pipet, drip the codeine (http://codeine.50g.com/info/codeine.html)/acetone mixture through the cotton. Follow this with a ml or two of clean acetone to get all the codeine (http://codeine.50g.com/info/codeine.html) from the pipet filter. Next, mix the acetone/phosphoric acid solution into the acetone/codeine (http://codeine.50g.com/info/codeine.html) base solution in a 50/50 ratio. As you stir the resultant misture, you will see the codeine phosphate quickly precipitate from the acetone as a sticky gummy mass. As you stir the solution, the final product should form a bolus on the stirring rod and look like a wad of chewing gum. Rinse the bolus in a small amount of fresh acetone and then smear it on a glass plate to dry. As the acetone evaporates, the codeine phosphate (CP) will appear to melt. This is because the CP is highly hygroscopic and is absorbing water from the air. Gently warm the CP in an oven to drive off the last of the acetone and then use a pipet or syringe to first drip water onto the CP, and then suck up the CP solution. You may now drink your product, or you can again reduce it to codeine (http://codeine.50g.com/info/codeine.html) base and extract it with chloroform if you prefer a much purer, powdered product.
Even after two acid-base extractions, I have gotten up to 93% of the available codeine (http://codeine.50g.com/info/codeine.html) from T3's with absolutely zero APAP in the finished product. If you choose codeine (http://codeine.50g.com/info/codeine.html) base as your final product, you can now easily turn it into even yummier alkaloids, but that is for another posting.
Sorry about the long cross-posting, but I believe in sharing information which will result in a purer (read: safer) final product. B.B. Welch