Bandil (Hive Bee)
06-21-02 17:10
No 323658
      DPT synth Q  Bookmark   

Hi!

Swim was dreaming of some legal DPT :) He followed TiHKAL to the letter, except he scaled up X5 with everything. The soln looked nice and reddish/brownish and kept getting darker by the hour. After 12 hours a LOT of white crystals suddenly precipated out of the soln and they just kept coming. At 40 hours reaction, the precipation has stopped, but the reaction vessel is quite full of pretty yellowish crystals. Now for the question:

TiHKAL does not mention precipation at this stage, but swim supposes that it is simply the diisoproylethylamine base, that has precipated as the iodide salt right? Swim was thinking og discarding the white sludge and exctracting on the remaing soln. Is this right, or should everything go into the A/B extraction?

Please resond ASAP, as swim is quite near the end of his dream!

Thanks a lot!

Regards
Peter
 
 
 
 
    Lilienthal
(Moderator)
06-21-02 20:46
No 323715
      Wrong!  Bookmark   

Wrong!

Although diisopropylethylamine is the stronger base, the precipitate may not be elusively diisopropylethylammonium iodide. Do a B or B/A/B extraction and have fun removing the diisopropylethylamine...
 
 
 
 
    Bandil
(Hive Bee)
06-21-02 22:05
No 323736
      and how would i remove the diisopropylethylamine?  Bookmark   

and how would i remove the diisopropylethylamine? Can it be distilled away?
 
 
 
 
    Rhodium
(Chief Bee)
06-22-02 01:36
No 323803
      Definitely.  Bookmark   

Yes, diisopropylethylamine has a much lower boiling point (127C at standard pressure) than DPT (145-155C at 0.08 mmHg).