Date: 19 Nov 1997 19:15:12 -0000 From: Satch Newsgroups: alt.drugs.chemistry Subject: Heroin manufacture revisited... Someone asked: >> Anyone know how to synthesize H from opium, or from the poppy plant? >> thanks. [...] >A fairly simple procedure was posted not long ago. The first >reference to "ammonia" should read "ammonium chloride"; otherwise >this is how they do it in Myanmar. (Also NaCO3 is used to basify >the ac. anhydride/heroin solution). [quote] >>to extract the morphine, heat the poppy extract in a solution of >>lime water. this will precipitate most the alkaloids and the >>meconoic acid as calcium mecanoate. The morphine and codeine >>will remain in solution. raising the pH of the solution to 9 >>with ammonia [NH4Cl] will precipitate the morphine and codeine >>and you can filter it out using very fine filter paper, and >>preferably running the filtrate through a millipore filter to get >>any you missed. morphine is unusual among plant alkaloids, being >>practically insoluble in most organic solvents. the free base is >>less soluble in ether than in water. codeine base is freely >>soluble in ether. washing the morphine with ether three times >>will remove most of the codeine. you now should have a morphine >>base that is better than 95% purity. to make it souble in water, >>simply dissolve it in a dilute solution of hydrochloric acid, >>adding more acid untill all of the solid is dissolved. if the >>solution is still slightly brown, it can be decolred with >>activated carbon. filter the carbon out and evaporate the water, >>and you have nearly pure morphine hydrochloride. >> >>if you want to make heroin, simply convert the salt back to the >>base using ammonia [NH4OH] like before and heat the base with >>acetic anhydride (three parts acetic anyhydride to one part base) >>under reflux at 85 degrees centigrade for six hours. distill off >>the excess acetic anhydride and mix the residue with water. >>raise the pH to 9 with ammonia [or, usually NaCO3] and heroin >>base will precipitate out. filter and convert to hydrochloride >>the same way as morphine. [endquote] >There is a few mistakes in your Heroin synthesis, and the Morphine >extraction, is actually part of an assay for Morphine, in Opium Tincture. >To do an extract from 500g of poppy straw, replace the lime water with about >100g of Hydrated Lime (50% Calcium Hydroxide), which is added to the hot >solution. The Calcium Hydroxide will react with the free acids in the >solution, but not breaking the salt bonds in the Morphine salts. [...] >The Calcium forms a sludge,which sinks to the bottom of the >vestal, carrying with it, the insoluble organic matter, leaving a >transparent black solution, containing the Morphine salts, which, >after concentration of the filtered so lution, the Morphine base >crystallises out, upon addition of conc Ammonia solution. Every procedure I've seen, including Beckett's, uses NH4Cl to precipitate morphine base from the calcium salt. Can ammonium hydroxide really be used interchangeably? (I don't see any reason why it can't, I just wonder why everyone says that ammonium chloride is to be used.) >In the Morphine to Heroin synthesis, the optimum amounts of >Morphine and Acetic Anhydride is weight for weight, you can use 3 >to 1 if you only have a few grams of Morph to play with, but you >will see what I mean when you compare the two different mixtures >under reflux. > >And the reflux temperature is irrelevant, the mixture will only >boil at one temperature, which is going to depend on the amounts >of base and anhydride you used, Acetic Anhydride boils at 139 >cercus, so the boiling point of the Acetic Anhydride and Morphine >mixture must be higher then 139 cercus. I don't even bother >checking the temperature, I just let it boil where it boils. But every account of the procedure says very specifically that it is *not* boiled. Hence the 85' C figure. Simmer, don't boil. >The rave about distilling of your excess Acetic Anhydride is >interesting, if you do this don't put it back in the original >bottle with your clean reagent, as this anhydride now contains >some Acetic Acid, you obviously didn't account for the one >molecule of water produced every time one molecule of Morphine is >acetylated which in tern will convert one molecule of Acetic >Anhydride to two molecules of Acetic Acid. > >I usually find it more convenient to neutralise all the anhydride >with 10%solution of Sodium Carbonate, (do not use Ammonium >Hydroxide to neutralise your anhydride, it's to strong, it will >strip your acetyl's back off your Heroin leaving you with >Morphine again), and you don't want that, do ya? [...] >The easiest way to obtain #!1 (brown rock Heroin), is after >making the anhydride mixture alkaline with 10% Sodium Carbonate >solution, extract three times with Chloroform (Diacetylmorphine >base: soluble 1g in1.5ml Chloroform. Merck Index 12th Ed), and >evaporate to dryness. Don't bother trying to make a salt out of >your heroin like you do with Morphine, it's just not the same. > >For one you can't work with Heroin in water or it will decompose >it to Morph and Monoacetylmorphine, Heroin has to be salted with >Hydrochloric Acid from Ethanol and Ether, don't bother [...] >it's to dangerous and it's easer to just use a couple of drops >of Vinegar or lemon juice in the spoon when you mix op your shot.