dormouse (Member)
04-20-00 02:32
No 108323
      PPA synth - quick, easy, cheap. -assholium  Bookmark   


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Author  Topic:   PPA synth - quick, easy, cheap. 
assholium
Member   posted 05-10-98 04:38 AM          
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Cheap and easy method of aminoalchogols production -
f.e. phenylpropanolamine, pseudo-ephedrine and so on, (and ring methoxylated too!!!)
preparation of PPA:

place in 1 l RGB flask 37 ml (35 g) isopropenylbenzene (bp 69C at 13 mmHg), then 250 ml of DMSO, add 15 ml H2O, and with stirring, add 106 g of N-bromosuccinimide in small portions durind 15 min. A yellow color appears when NBS is added, and by the time the addition is complete, the color is bright-orange. Durind the addition temp rose up to 50 C. Stir another 15 min, then pour into 1 l of cold water and 3-5 times extract with 100-ml portions of ether. The combined etherial extracts washed water, then NaCl soln, extract dried over MgSO4 and ether was distilled off. Obtained 70 g of yellow oil PhCH(OH)CH(Br)CH3. Yield almost quantitative.
Ref: Organic Syntheses, vol 59, p.16.


dissilve this oil in 100 ml of methanol. Saturate 400 ml of methanol with ammonia at -10C (bubble ammonia until volume grows to 50% - up to 550-600 ml). Mix methanolic soln of bromohydrine with ammonia soln, place it in sealed bomb and heat at 110-120C 4-5 hrs. After cooling open it carefully (ammonia evolution!) poll in 1 l glass (carefull, please - mixture foamy as freshly-opened shampagne) and allow main quantities of ammonia fly out at slowly heated water bath. Distill of methanol and obtained semi-cryst oil dissolve in 300 ml of 20% HCl. Wash milky soln twice with hexane, basify and extract PPA with methylene chloride (3x100 portions). Dry with NaSO4, and remove solvent. Result - about 42 g of oil, cryst on chilling with mp 53-55C.
Conversion of isopropenylbenzene - PPA is 92%. Not bad, I think.


 
Rhodium
Administrator   posted 05-10-98 05:55 AM          
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What about Propenylbenzene => Pseudonitrosite with N2O3 or NaNO2, react it with Ac2O to give the alpha-acetoxy-beta-nitro phenylpropane. Reduce the nitro group and hydrolyze the ester to give PPA. I'd guess the yields are at 50-75% total, but a lot easier than your version.
 
Rhodium
Administrator   posted 05-10-98 05:55 AM          
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What about Propenylbenzene => Pseudonitrosite with N2O3 or NaNO2, react it with Ac2O to give the alpha-acetoxy-beta-nitro phenylpropane. Reduce the nitro group and hydrolyze the ester to give PPA. I'd guess the yields are at 50-75% total, but a lot easier than your version.
 
David
unregistered   posted 05-11-98 03:02 PM           
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Rodium, you nerd. Make METH out of propenylbenzene, not dexatrim!!
*smack*
 
David
unregistered   posted 05-11-98 03:02 PM           
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Rodium, you nerd. Make METH out of propenylbenzene, not dexatrim!!
*smack*
 
Rhodium
Administrator   posted 05-11-98 03:57 PM          
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Hey David, assholium did just the same, I just improved his method. And besides, I don't want meth, U4EUh is probably better 


Rhodium
Administrator   posted 05-11-98 03:57 PM          
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Hey David, assholium did just the same, I just improved his method. And besides, I don't want meth, U4EUh is probably better 


Labrat
Member   posted 05-12-98 09:55 AM          
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He Rhodium, why make methylaminorex if aminorex is more potent? Just read "Future Synthetic Drugs of Abuse". You can find it at: http://www.hyperreal.org/drugs/misc/future.html. 
Besides, using the cyanogen bromide process the yields are higher when making aminorex instead of methylaminorex. Does anybody on this board know why aminorex is no longer a registrered medicine? No, it's not the fact that it's addictive, it's got to do with the toxicity you get from using this compound for a long period of time. I can recall vaguely that some sort of longue disease can be induced by long-term use of aminorex. But that doesn't matter here, cause we are all casual users, right? Sure...
 
Labrat
Member   posted 05-12-98 09:55 AM          
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He Rhodium, why make methylaminorex if aminorex is more potent? Just read "Future Synthetic Drugs of Abuse". You can find it at: http://www.hyperreal.org/drugs/misc/future.html. 
Besides, using the cyanogen bromide process the yields are higher when making aminorex instead of methylaminorex. Does anybody on this board know why aminorex is no longer a registrered medicine? No, it's not the fact that it's addictive, it's got to do with the toxicity you get from using this compound for a long period of time. I can recall vaguely that some sort of longue disease can be induced by long-term use of aminorex. But that doesn't matter here, cause we are all casual users, right? Sure...
 
Rhodium
Administrator   posted 05-12-98 02:28 PM          
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Potency has a very low ranking by me. The qualitative experience is a lot more important.
 
Rhodium
Administrator   posted 05-12-98 02:28 PM          
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Potency has a very low ranking by me. The qualitative experience is a lot more important.
 
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