bbell (Newbee)
03-19-03 20:07
No 419288
      having a problem with L.A. extraction  Bookmark   

following is verbatum from journal of biological chemistry vol.104(3)547-51(1934)by W.A.Jacobs & L.C.Craig.
In preliminary experiments it was found that crystalline ergotinine could be refluxed as a suspension in 6 % aqueous potassium hydroxide without appreciable alteration. This apparent resistance proved to be due to its insolubility. If ergotinineis first rapidly dissolved in methyl alcoholic KOH and the solvent is emmediately removed at low temp. and pressure, a resinous residue remains. When this residue is heated with aqueous alkali, as described later, it gradually dissolves with the liberation of ammonia due to cleavage of the amide group of ergotinine. Naturally, no ergotinine could be recovered from this reaction mixture. Futhermore, none of the base, ergine, could be detected on direct extraction of the alkaline hydrolysate. However, a new substance was obtained in good yield on gentle acidification, which possessed both acid and base properties and which we have named lysergic acid. This paper gave the production of d-L.A. hydrate

From J.Biol.Chem.vol.112Pages 245-53(1936)same authors.
They discribe the alkaline hydrolysis of ergotamine tartrate and ergoclavine to give d-lysergic acid hydrate. These processes are again more complicated that most other published reports. Namely A. Shulgin who states A solution of 6.7 g.KOH in 100 ml. water,under an inert atmosphere magnetically stirred 10 g. ergotamine tartrate added. Reflux
4 hours acidify to PH 3 with H2SO4 to precipitate D-L.A.hydrate.
  Which of these procedures works best? or at all?