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	Posts 1 - 19 of 19	Subject: P2P via German Patent

	Bwiti (Hive Bee) 02-16-01 19:27 No 173860		P2P via German Patent	Bookmark Reply
			What's up folks?! Last night I was poking around a patent database whe I ran into an interesting P2P synth. Here's why I think this patent would be useful to evil chemists: Someone can scrounge up a shit-load of pseudoephedrine from cold pills, or ephedrine from ephedra powder, but the hard part is obtaining RP. Who wants to scrape RP off of match-books? Fuck that! I did my best to translate the patent, but it still needs work..Anyone here good with german? ------------------------------------------------------------ ------------------------------------------------------------ Procedure for the Production of Phenylacetone Patent # :  DE3200232 (addition for patent application P 30 26 698.9-42) The invention concerns a new arrangement of a procedure for the production of phenylacetone. The subject of the principal patent (patent application P 30 26 698,9-42) is marked a procedure for the production of Phenylacetone from Ephedrinen by sulfuric acid, by the fact that one executes the conversion to 50 to 70 of %iger acid with 150 to 155*C and to presence from 0,02 to 0.5 % zinkchlorid as catalyst and that one out-distills the Phenylacetone by water vapour from the reaction beginning. It was now found that one can execute the conversion also in presence from 0,05 to 0.3 % of another metallchlorides in place of 0,02 to 0.5 % zinkchlorid. When other metallchloride are suitable Eisen(III) chloride and in particular aluminum chloride, boron tri fluoride and Titan(III) chloride, which are used as Lewis acids in organic chemistry. The concentration of the sulfuric acid is selected in such a way, which amounts to their content in the reaction mixture 50 to 70 thread %. The reaction runs particularly well with a sulfuric acid content from approximately 60 %. For the distance of the Phenylacetone from the reaction mixture water vapour is initiated into the mixture, which removes the developing Phenylacetone immediately from the mixture. The received distillate is extracted with toluol and the excerpt is abdestilliert. Thus one receives Phenylacetone, which is pure over 99,5 % too. When Ephedrine come Ephedrin, Pseudoephedrin, Norephedrin and Norpseudoephedrin as well as Bis(1 phenyl 2 methylamino propyl 1) ether in consideration, whereby the reaction for such Ephedrine is particularly important, gave no direct use for it so far ((-)-pseudoephedrin, (-)-norpseudoephedrin). The Ephedrine preferably becomes in a weight ratio of approximately 1: 1 to 1: 10, preferably 1: 2 to 1: 5 with the acid transferred. The yields, which will receive with the new procedure, are with 80 %. the procedure run with relatively high rate. A further advantage of the procedure consists of the fact that it can be continuously executed. Thus one can let a hot aqueous solution of the Ephedrins flow into the hot acid, whereby the Azeotrop Phenylacetone/Wasser abdestilliert continuously. Here it is only necessarily, the developing amine salt, e.g. sulfatesulfate sulfate, to remove occasionally. The use of the mentioned metal halides in place of ZnCl2 offers advantages regarding environmental protection, because this are more harmless and do not disturb the biological reduction of the waste water. Example 1 1025 g 75 %ige sulfuric acid are shifted with 2 g AlCl3. In it 426 g (= 2.58 mol) are solved Ephedrin or Pseudoephedrin cousin with 50 to 100*C. Subsequently, the mixture on 145 to 150 is heated up *. With 125*C water vapour in moderate current is initiated for better mixing. With 145*C one strengthens the introduction and distills in the period of 2 1/2 to 3 Studen the Azeotrop Phenylacetone/Wasser over. From the distillate one isolates by toluol extraction a raw Phenylacetone, which is free from Propiophenon. After distillation over a short Vigreux column one receives Phenylacetone, purity to 270 g (78%): 99.8 %. One keeps similar from Norephedrin or Norpseudoephedrin Phenylacetone in a yield from approx. 80 %. Example 2 In 1000 g 79 of %iger sulfuric acid 100 g become (-)-Pseudoephedrin-cousin solve, whereby the H2SO4 - concentration to 65 to 66 % it is adjusted. This solution is given in 2 the 1 three-neck piston, shifted with 4 g AlCl3 and heated up to 125 to 130*C. By injecting water vapour one increases the temperature on 145 to 150*C and leaves from now to continuously with a rate of approximately 1 to 5 g/min 70 to 90*C a warm a solution of (-)-pseudoephedrin (cousin) into 79 of %iger sulfuric acid (weight ratio 1: 1) flow over a steam-heated dropping funnel. The Phenylacetone turns into thereby as Azeotrop and similar to example 1 is regenerated. After in each case 4 Studen the reaction is interrupted for 5 minutes and removed at flow of the 5 minutes so much sulfuric acid that the output volume is re-created. Afterwards the reaction is continued. The taken sulfuric acid can be reused after removing from the methyl ammonium methylammoniumhydrogensulfat developed during the conversion. The yield at Phenylacetone amounts to 76 %. Example 3 1350 g 79 %ige sulfuric acid become in a reaction piston submitted and under agitating with 590 g 95 %igem (+)-Ephedrin shifted. 10 ml 18 %ige TiCl3 become subsequently, - solution admitted and the mixture with 125*C beginning and to 145-155*C rising with water vapour distillate caught, from which by toluol extraction 358 g Phenylacetone were isolated. From it 335 g = 73.6 were received by fractionated distillation over a Vigreux column % Phenylacetone, to purity: 99.5 %. Example 4 In 1350 g 79 of %iger sulfuric acid under agitating 561 g d-l-Ephedrin (99-100 %ig) are solved, with 15 g BF3 - glacial acetic acid solution (10 %ig) transferred and to 125*C heats up. One injects water vapour and increases the temperature thereby on 145-155*C whereby developed Phenylacetone is over-driven. After approx. 6 1 water vapour distillate was caught, splitting is terminated. One isolates 386.4 g Phenylacetone from the distillate by toluol extraction and distillation. From this 367 g (80.6 %) are received pure Phenylacetone. Example 5 To 400 kg of 60 of %iger sulfuric acid in a distillation apparatus 500 kg of 80 %ige sulfuric acid are course-pumped. Into this mixture 400 kg become under Rueren (-)-pseudoephedrine (60 %ige) and 1.5 1 aluminum chloride solution (30 %ig) entered. One heats the reaction mixture on 125-130*C and initiates dan under further temperature increase on 145-150*C water vapour, whereby a mixture of water vapour and Phenylacetone abdestilliert. After approx. 2000 1 water vapour distillate was caught, one terminates distillation. From the distillate the heavy phase, consisting of Phenylacetone, is separated and the aqueous phase is extracted with approx. 400 1 toluol. The separated Phenylacetone and the toluolische excerpt are combined and concentrated by distillation. The remaining arrears are afterwards fractionated distilled. One receives pure Phenylacetone to 155 kg (80 %). ------------------------------------------------------------ ------------------------------------------------------------ Peace!   Normalement je suis droit, mais je veux vraiment embrasser " Mulder " (du X-Files)! Il est chaud!
	terbium (Hive Addict) 02-17-01 07:42 No 173956		Re: P2P via German Patent	Bookmark Reply
			That is a great find now that rP is so hard to get. P2P from OTC reagents! The meth would be racemic but it sure beats scraping matchbooks to get rP.
	foxy2 (Hive Addict) 02-21-01 12:35 No 174715		Re: P2P via German Patent	Bookmark Reply
			How would one produce anhydrous Lewis Acids? Can hydrated FeCl3 be dehydrated in any reasonable way? Would anhydrous HCl gas and dry iron fileings be the way to go? Foxy Out Do Your Part To Win The War
	uemura (Hive Bee) 02-21-01 12:53 No 174719		Re: P2P via German Patent	Bookmark Reply
			Would anhydrous HCl gas and dry iron fileings be the way to go? Think so, at least Gattermann-Wieland uses this to get anhydroneous AlCl3 from Al and HCl Carpe Diem
	PolytheneSam (Hive Bee) 02-21-01 16:34 No 174755		Re: P2P via German Patent	Bookmark Reply
			You can get anhydrous FeCl3 from some electronics companies.  Its mixed with water and used to etch printed circuit boards.  I have a mail order catalog around somewhere that has it in.
	terbium (Hive Addict) 02-22-01 15:49 No 174948		Re: P2P via German Patent	Bookmark Reply
			But according to the patent you would not seem to need anhydrous materials. Steam is injected into the pot as the reaction is proceding in order to steam distill of the P2P as it is formed. The patent even talks about doing this as a continuous process where ephedrine is a also continously added. It seems to me that hydrated aluminum chloride should work just fine. Also, zinc chloride in most any form should work.
	jim (Newbee) 02-23-01 09:16 No 175060		Re: P2P via German Patent	Bookmark Reply
			I found a similar article quite awhile ago, but it didn't post any yields.  I am glad to find out that the yields are respectable.  My suggestion is:  Don't steam distill, it will complicate things.  Take the sulfuric acid and ZnCl2, put into flask.  Heat and add the crude ephedrine pills.  The ephedrine turns into P2P, the fillers are chewed up.  Extract with nonpolar like toluene after reaction has run its course and cooled down.  Use P2P in any fashion you like to get racemic amphetamines.
	elfchemist (Newbee) 02-26-01 01:06 No 175531		Re: P2P via German Patent	Bookmark Reply
			Let BieneMaja have a look at it, he would be able to help with any German translations. pharmaceutical companies, you've got to love them.....
	Bwiti (Hive Bee) 02-26-01 02:25 No 175539		Re: P2P via German Patent	Bookmark Reply
			"Don't steam distill, it will complicate things.  Take the sulfuric acid and ZnCl2, put into flask.  Heat and add the crude ephedrine pills.  The ephedrine turns into P2P, the fillers are chewed up.  Extract with nonpolar like toluene   You're right about the steam-distillation..Fuck that! After extracting, the P2P will probably be a little dirty, but there is plenty of info out there regarding it's clean-up.   "crude ephedrine pills"? If I was going to do this reaction, I'd definately do an A/B extraction on the pills. They contain loads of fillers that could fuck-up the extraction of the P2P and create an emulsion. Peace!   Normalement je suis droit, mais je veux vraiment embrasser " Mulder " (du X-Files)! Il est chaud!
	BieneMaja (Hive Bee) 02-26-01 13:42 No 175639		Re: P2P via German Patent	Bookmark Reply
			In reply to: ‘Let BieneMaja have a look at it, he would be able to help with any German translations.’ Gee, I had. When Bwiti finishes the last grammar and style check I’m sure he’ll post it immediately. In reply to: ‘My suggestion is:  Don't steam distill, it will complicate things. Take the sulfuric acid and ZnCl2, put into flask.  Heat and add the crude ephedrine pills.  The ephedrine turns into P2P, the fillers are chewed up. Extract with nonpolar like toluene after reaction has run its course and cooled down.[..]’ although example 5 mentiones that very crude ephedrines, in this case 60% pseudo and 40% gakk, can be used with good yield (80%) swib wouldn’t recommend it. The cleaner the starting material the easier everything goes. Don’t ask me in which way povidone reacts with the sulfuric… and don’t forget that meAmsulfate/hydrogensulfate is also produced and it would be stupid to combine this nice stuff with unknown gakk. I like steam destillation and wouldn’t skip it. Does anybody know how resistable p-2-p is against hot 60-70% H2SO4? And of course, if one of the products is removed it forces the reaction in one direction: [C]*[D] ------- = K  K = const (if temp. is const.) [A]*[B] should be familiar to everybody, shouldn’t it? per aspera ad astra
	terbium (Hive Addict) 02-26-01 22:52 No 175694		Re: P2P via German Patent	Bookmark Reply
			Methamphetamine via Leuckart-Wallach (refluxing P2P in formic acid/n-methylformamide) certainly produces a lot of tar. Steam distillation of the P2P as it is formed would certainly help get it out of the reaction pot before it could be turned to tar.
	BieneMaja (Hive Bee) 03-02-01 10:55 No 176160		Re: P2P via German Patent	Bookmark Reply
			edited cause it is already in the sequel! I have to mention that although the Knoll AG ™ is a german company (or was it at least´in 1982) their patent was written in such a bad german (concerning grammar and stylistic abilities) that I transformed some sentences without changing ther content. Otherwise it would have been impossible to me to write a readable text. although the main content is deleted this is still offered (as a little 'pay back-what-you've-got-out-of-it'): If anyone has any question to this or another german ‘synth’ them semd me a pm and I’ll try to answer it. ea vita est via in caelum (seneca) [this life is the way to heaven]
	LaBTop (Daddy) 03-02-01 15:29 No 176212		Re: P2P via German Patent	Bookmark Reply
			Nobody seemed to have noticed that I already had it translated and put it up there in the first sticky thread, "The Sequel". Biene Maja, could you compare my translation of Bwiti's post (I did not translate from the patent which I didn't see, but merely cleaned up the wicked textpeaces, as good as I understood was what meant) to your translation? Then if there is anything to edit, I will do that and change that up there. It's a fine bigscale method. I think I remove all those sticky threads, nobody seems to read them with attention to details. Saves me a lot of work, can concentrate on other things then. LT/ WISDOMwillWIN
	BieneMaja (Hive Bee) 03-02-01 17:36 No 176232		Re: P2P via German Patent	Bookmark Reply
			Nobody seemed to have noticed that I already had it translated and put it up there in the first sticky thread, "The Sequel". Biene Maja, could you compare my translation of Bwiti's post (I did not translate from the patent which I didn't see, but merely cleaned up the wicked textpeaces, as good as I understood was what meant) to your translation? Then if there is anything to edit, I will do that and change that up there. It's a fine bigscale method. shame on me i read 'the sequel' some days ago in the newbee forum and did not expect you to work so fast. your tranlation is without a mistake and has a much better english of course. i sent my trnslation to bwiti some days ago but it didn't arive him as it should your enzyclopedia saves a lot of bees a lot of time, don't remove them only because some of us aren't worth your work ea vita est via in caelum (seneca) [this life is the way to heaven]
	psychokitty (Kitty-KrZ / Eraser) 03-04-01 15:31 No 176503		Re: P2P via German Patent	Bookmark Reply
			You can also get ferric chloride from certain photographic chemical supply houses--the names of which I'll refrain from mentioning here.  Also, according to one article that I have, P2P can be synthesized from ephedrine or pseudoephedrine by heating with hydrochloric acid under pressure at elevated temperature. --PK
	foxy2 (Hive Addict) 03-04-01 22:42 No 176615		Re: P2P via German Patent	Bookmark Reply
			Thats great psycho And i have an article that says X can be made with dog shit and peanut butter. Why don't you grace us with that reference? Do Your Part To Win The War
	firecracker (Newbee) 03-07-01 08:53 No 177124		Re: P2P via German Patent	Bookmark Reply
			Some questions if I may: 1) Is propiophenone the major secondary product of this reaction?  The text seems to imply that at least some is produced. 2) I would assume that propiophenone doesn't form an azeotrope with steam, and thus won't distill across?  This would make steam distillation preferable, since fractional would be damn near impossible because of the close bp's. 3) I would think that any propio mixed in with the ketone would aminate as well, giving 1-phenyl-1-methylamino-propane??? (Is this correct?) Any have any refs on that compound? Thanks for any input... Snap, Crackle, Pop
	BieneMaja (Hive Bee) 03-09-01 02:45 No 177441		Re: P2P via German Patent	Bookmark Reply
			Some questions if I may: of course 1) Is propiophenone the major secondary product of this reaction?  The text seems to imply that at least some is produced. the patent isn't very clear at this point, maybe they just want p-2-p and do not care about the byproducts. (which wonders swib, cause the chem industries (knoll ag) are normally very interested in synthetic routes producing no byproduct which isn't usable.(strange sentence) i mean sometimes it will be cheaper to follow a 75% yield route instead of an 96% route where those 4% are totally worthless for them. figure it out yourself this reaction isn't that hard to understand 2) I would assume that propiophenone doesn't form an azeotrope with steam, and thus won't distill across?  This would make steam distillation preferable, since fractional would be damn near impossible because of the close bp's. did you read lt's translation??? the steamdestillation removes the p2p uot of the reactionmixture/-vessel (has been discussed in this thread) and fractionated ditillation is a powerfull cleaning method. if bp's of two substances are so close tha normal distillation would fail, fractionated dest. may work. ther are formulas with which you could figure out how many 'normal' dest you would have to make using not a vigreux coloumn but a normal liebig/west/.. condensor I would think that any propio mixed in with the ketone would aminate as well, giving 1-phenyl-1-methylamino-propane??? (Is this correct?) Any have any refs on that compound? i dunno, but thats out of question with this procedure, cause the product is free of propiophenon. ea vita est via in caelum (seneca) [this life is the way to heaven]
	firecracker (Newbee) 03-09-01 09:00 No 177473		Re: P2P via German Patent	Bookmark Reply
			Thanks BM, Let me restate some things for clarity: I understand the steam distillation. But I guess I don't understand why they mention propio at all. If it is a side product it would seem like a pain to clean out, even using fractioning. That statement in the text about isolating propio free stuff with toluene doesnt make sense to me.  According to the Mercks I'm looking at both are soluble. My assumption is that there isn't any propio produced at all, but I can't prove it conclusively. I would just like to know why the author mentions it. To be honest I'm not that interested in this reaction. Tweakin just ain't my thang. I thought I saw a discrepency and figured I'd ask the question. Never learn if you don't ask... Snap, Crackle, Pop

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