Ephedrine Free base,using NaOH,xylene and distilled,deionized water - the Hive BB

Ephedrine Free base,using NaOH,xylene and distilled,deionized water

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Author	Topic: Ephedrine Free base,using NaOH,xylene and distilled,deionized water
Worlock Hive Bee	posted 01-24-2000 11:38 AM Ephedrine Free base(E-FB), using NaOH, xylene and distilled, deionized water ----------------------------------------------------------------------------------------------------------------------------- 480 tablets, of 60 mg, Pseudoephedrine HCl, O.T.C.B. brand, were placed in a blender and ground to powder. The powder was placed in a 1000 ml flask with enough distilled, deionized water (D-D-water) to cover the powder by 3 inches. This was well shaken, and placed on a warming tray. The D-D-water was purchased as distilled, then run through a small Britta water filter unit. After a few hours the flask was emptied and rinsed into a vacuum Buchner, the mixture was filtered repeatedly , until clear. The filtered water / ephedrine mix was placed in a separatory funnel along with 200 ml of xylene, To the funnel was added 500 ml of a 20% NaOH solution. Immediately a cottage cheese appearing basic amine rose to the top. Additional xylene was added until the ephedrine became sooth and creamy in texture, This was shaken and allowed to sit for 45 minutes. The lye/water layer was removed and set aside. Multiple washes of the xylene / ephedrine were preformed using D-D-water, this was repeated until the wash water came back clear. After the xylene / E-FB mix was allowed to separate undisturbed for 30 minutes, the remaining water was flushed and the Ephedrine was placed in a bowl, on a warming tray, with a hair dryer, on low, blowing over it. Three hours later white crystalline Ephedrine free basic amine was obtained. There was no xylene odor, only a very slight ephedrine odor. The crystals were very mildly bitter to taste. The crystal was sifted and weighed . From 28.8 gms of E-HCl (mw=202) , 20.0 gms of E - FB (mw=167) were obtained 28.8 / 202 = 0.14 moles E-HCl 20.0 / 167 = 0.12 moles E -FB 0.12 / 0.14 x 100% = 86% yield by mole 20 gms of E-FB is equivalent to 24 gms of E-HCl The fillers were tasted and were slightly bitter. They contained enough E to be washed again in the next batch. Also clumps of ephedrine were seen floating on top of the wash water. The errors at this point are: 1) A failure to rinse the fillers with fresh D-D-water after repeated filtering of the Ephedrine / water mixture. 2) Over running some of the E-FB in with the wash water . The wash water was placed back in the separatory funnel with 50 ml of xylene and 150 ml of lye solution, from which more E-FB will be extracted. Satisfied with the outcome, at this point, it was determined that an additional, 60 gms of E-HCl would be treated in this manner before reacting. Gotta run to the store , More to come, soon ! . ------------------ Worlock *Web Page*
ChromYum Hive Bee	posted 01-24-2000 05:19 PM Hey Worlock not workin today? Or are ya? Does the Britta de-ioniZe water? Is that hardware store xYlene? And what is OTCB brand? Did you pull down all your stained-glass windows again? Or are you going to reaction with your new electrothingy?
mrr pyrex Hive Bee	posted 01-25-2000 03:03 AM Yeah I was wondering about that de-ion thing too?? I wouldn't appear that a water filter would be able to de-ion the water, but I could be wrong. And seeing as how I've never tried de-ion water I don't know, but I would be willing to bet that de-ion water would behave differently then just distilled water, when doing extraction. Pyrex out
CHEMMAN Hive Bee	posted 01-25-2000 03:20 AM Android once posted his preference of Xylene over toluene.Something about emulsions?? Now that you have used both what is your opinion.Has anyone beaten povidone and got it out before it creates havoc at AB time? New Oz polymer pills wont AB up front , but the polymer does settle out in methanol. 2 or 3 extractions needed.Povidone is also in there, but a steam dist after the reaction fixes it nicely.Thanks for the report
aqua-girl Hive Bee	posted 01-25-2000 05:48 AM triple-distilled is usually pretty clean as far as minerals kicking around. unfortunately most distilled we use is stored in big copper vats out of metal stills. There is a product for the aquarium market called the Tap Water Purifier made by Aquarium Pharmaceuticals that is a mixed bed DI cartridge. Some exchange resins can be recharged. Also, you can call your local culligan/us filter and get the exchange resins yourself. I took 4 TWP cartridges, put them in flow post-RO (Spectrapure), then it went through anion, cation, carbon, and then a special resin designed to remove silicate (big deal in aquariums). Or you could just pop the $$ down for a milli-q lab unit
Worlock Hive Bee	posted 01-25-2000 01:49 PM Exactly as Aqua girl describes it, the distilling vats are metal especially copper, Most all distilled water has ionic copper. the Britta claims it will remove this. I am not very trusting of distilled water, I'm sure it is distilled, in a fashion, but lower boiling point contaminants are going to come over with the water distillation. You know the distributers are not bustin' ass to deliver a super clean d-water. They just grind it out, so it has not too much salt. In Chem labs, the stuff is distilled several times from glassware then run through resin unit to remove certain ions. The Britta(yes, I did just purchase Britta stock options), will remove most organic and metalic contaminents, with filtration and activated carbon, I would guess there is a bit of resin in them also. **************** OTCB is the DEA's prime quality brand of pseudoephedrine, they are in the business, you know. OTCB Clearwater, Fl 33762 1-800-634-PILL (7455) ************* Xylene(xylol)- micro circuitry I still prefer Toluene, xylene takes longer top separate from water ********************* I am not involved in that particular bogus non-functioning Electrothingy, although there are several electro catalytic units that will work. ******************** Yes the povidone is beatable, The steam distilling sounds great, and is an approach that is new to me. By adding a step in the A/B, povidone can also be removed. After filtering the alcohol / ephedrine solution, hit it with a Base to make the E freebase the povidone moves into the non-polar along with the E, and becomes a gross lumpy solid. Heat the mixture to boiling, this coagulates the povidone and locks it in the solid phase. The heat makes the E dissolve better. Pull the big globs of povidone out of the solution with a fork, then strain out the smaller clogs, then filter the remaining funk, and your free of povidone. If you dry it, it will form a minute amount of off-white powder. The wild thing about povidone is it tries to parallel the density of the surrounding solution. But the basic soplution tweaks it good, by making it a semi-solid then use heat to lock it in the solid form. Ther steam distilling is somewhat similar.
CHEMMAN Hive Bee	posted 01-25-2000 10:11 PM Thanks Worlock .I am now a follower of steam dist.If you have any questions , I am most willing to offer my learnings as you have offered yours.I tried it without filtering the RP first, and was a bit slow to distill. Just dreamt of a good pill cleanup, followed by Rp and I reaction.Added water and filtered contents.. Added ice and Ph to approx13.Povidone is evident. Steam oil and water across .Ph to 7 and evap .Nice clean stuff. Then I awoke very happily.
CHEMMAN Hive Bee	posted 01-25-2000 10:45 PM Also as the steam dist goes on, the povidone seems to go into the lower aqueous layer. The steams heat seems to break it down . whatever happens it does not hinder yield. After the RP I Rx, my aqueous contents seem to be in two layers ?? With several changes, this has always been the case. Any ideas??
Android PimpBee	posted 01-26-2000 09:31 AM Glad to see you're still knockin' about, Worlock! Keep up the good work, Teacha! BTW. DD tell ya we finished the Hive Song? Used your verses verbatim.(Don't fix it if it ain't broken, right?) I've wasted enough of your time, W. You ladies can return to your research now!
aqua-girl Hive Bee	posted 01-26-2000 11:38 AM You mentioned wacking the stuff with an oxidizer in some thread... sometime. Did you try it? I'm thinkin' about tossing a bunch o' pills into a blender with some dh2o or alcohol, tossing in a pinch of kmno4 and letting it spin for awhile, then basing it out. if methcathinone reduces via HI/P, then any ephedrine that flips to cat won't be a problem.... of course, I'd hate to nuke a batch of pills and end up with busted up ephed molecules all over the place
(Lloyd) Hive Bee	posted 01-27-2000 04:53 PM One of the advantages of starting in alcohol is that it does not seem to present this particular problem. the Honorable Mr. W. and I were discoursing about povidone once and speculated or noted that it also coagulates in the NP under freezer conditions. The Xylene dissolves the LEAST water (occult water) in it among the "leading" NP's: thus making it most attractive for dry gas precipitation. On the other hand, if you fling in HCl, shake like hell, and evaporate the water phase, and do the acetone boogie with the remnants, who cares. (Lloyd)
Android PimpBee	posted 01-28-2000 04:45 PM It's the pest again! Worlock, email me at android2000@mailcity.com and I'll send you a copy of the Hive song. Thanks, partner! ------------------ "WARNING: AvoidAndroid! Hesucks!"

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