Tezcatlipoca (Stranger)
07-23-02 18:53
No 336158
      Al/Hg redn. of 2,5-DMP2P w/NH3  Bookmark   

I realise it would be low, but what kind of yield could bee expected from Al/Hg redn. a la Osmium (../rhodium/chemistry /alhg.osmium.html) of 2,5-dimethoxyphenylacetone using aqueous ammonia?

Thanks in Advance,
Tezcatlipoca
 
 
 
 
    Vibrating_Lights
(Hive Addict)
07-23-02 20:00
No 336176
      rxns  Bookmark   

The problem with these reactions is that the amphetamine product is a primary amine which will then react with more of the ketone.  For best results with an Otc approach would be to make the Oxime with hydroxlamine then reduce with Al/Hg in AA/EtOH yeilds warry with the ring substitution pattern.  How did you make the ketone??????  If you do attempt the reduction in Ammonia I would suggest Using Alcohol gassed to saturation with NH3.  The higher the concentration of amine the lower the yeild loss due to amphetamine reacting with ketone.  Good luck. hydroxlamine can be made from NitroMethane and HCL(UTFSE)
VL_
 
 
 
 
    Tezcatlipoca
(Stranger)
07-23-02 20:27
No 336184
      re: rxns  Bookmark   

Thanks V_L. If Tezcatlipoca were actually doing this rxn, he would probably use the Leuckart (if he went via the P2P at all). I just wondered what the probable yields for this rxn would bee for research purposes. 25DMP2P was made by Fe/HCl redn. of 25DMP2NP.

Thanks,
Tezcatlipoca
 
 
 
 
    Rhodium
(Chief Bee)
07-23-02 21:16
No 336189
      Writeup please  Bookmark   

Tez: Could you give us full reaction details of your preparation of 2,5-dimethoxyphenyl-2-nitropropene and 2,5-dimethoxyphenyl-2-propanone, please, with amounts, boiling points, yields and all?
 
 
 
 
    Vibrating_Lights
(Hive Addict)
07-23-02 22:53
No 336213
      do the oxime  Bookmark   

Make the oxime.  Antibody reported good yeilds with most oximes
VL_
 
 
 
 
    Chromic
(Synaptic Self-Mutilator)
07-23-02 22:57
No 336214
      yeah  Bookmark   

3,4,5-tmp2p formed the oxime in OK yields for me... and seemed to reduce alright. I'd expect 2,5-dmp2p to go alright as well..

It will certainly go better than the Al/Hg with NH3.
 
 
 
 
    Sunlight
(Pioneer Researcher)
07-24-02 15:03
No 336536
      CTH  Bookmark   

If you have the ketone, ammonium formate and Pd/C you can get good yields with the CTH reductive amination. See in the Novel Discourse.
 
 
 
 
    Tezcatlipoca
(Stranger)
07-26-02 20:33
No 337429
      Re:  Bookmark   

Thanks all :D

Rh: Will post full writeup when synth is complete. Yield of nitropropene and p2p were both ~75%.

- Tezcatlipoca -