n00dle (Hive Bee)
09-20-04 06:22
No 532275
      hydrolysis questions     

methanol/NaOH hydrolyses ergot alkaloids to lysergic acid, but in crappy yeilds/lots of isomer.

methanol/KOH hydrolyses ergot alkaloids to lysergic acid in decent yeilds with a portion of isomer.

In a thread here, an LSD chemist posed using potassium metal refluxed in ether/methanol to eperimize iso-lsd, in fantastic yeilds with little letover isomer.

 Since in the previous reactions, the same relative agents (naoh/koh) are used in eperimization procedure as they are in the hydrolysis procedure, is it safe to say that the K/methanol/ether (potassium methoxide) will hydrolyse the precursor? (since we already know it will eperimize the product)
 
 
 
 
    hest
(Hive Adickt)
09-20-04 07:21
No 532284
      Wather     

You need some wather to doo the hydrolyse (therby the name)
 
 
 
 
    n00dle
(Hive Bee)
09-21-04 16:24
No 532493
      1.0g of ergotinine was dissolved in 20ml of...     

1.0g of ergotinine was dissolved in 20ml of N-methyl alcoholic KOH and the methanol was removed at once by distillation at low pressure. The residue was treated with 20ml of an 8% aqueous solution of KOH and the mixture was heated on a steam-bath for 1 hour. A stream of nitrogen was passed through the flask during the heating and basic volatile material from the reaction mix was collected by passing the gas through a solution of dilute HCl acid.

Where in that does it show water? Maybe swim should reask his question. In regards to NaOH/KOH, where it is the same method for eperimization and hydrolysis in lysergic acid preperations, could the novel potassium metal/anhydrous methanol/ether method of eperimization be somehow used or modified to be used as the hydrolysis procedure? Eperimization and hydrolysis using NaOH/KOH have similar yeilds, so SWIM is hoping that the K/methanol/ether eperimization method that yeilds something like 95% can be somehow used for the hydrolysis prep to get better yeilds over the existing best method, using tetrabutylammonium hydroxide, which isn't watched, but is known for specific use in lysergic acid preps and could ring some sort of suspicion bell. (plus if it can be modified, it'd supercede the tetrabutylammonium hydroxide method in terms of yeild.)
 
 
 
 
    hest
(Hive Adickt)
09-22-04 08:31
No 532640
      Wather     


The residue was treated with 20ml of an 8% aqueous solution of KOH




Where in that does it show water?



Iff It's a joke I don't get it crazy

 
 
 
 
    n00dle
(Hive Bee)
09-24-04 17:30
No 532991
      Okay. Call SWIM really stupid, but i just...     

Okay. Call SWIM really stupid, but i just don't get it. Can the K/ether/methanol eperimization procedure of lsd synths be used or modified to be used for the hydrolysis section, is what SWIM is asking. (So we can get even higher yeilds of hydrolysis rather than tetrabutylammonium hydroxide/KOH/NaOH on ergot alkaloids)