My fellow bees, I just recived a note from a person who wrote this:
Many years ago I would buy egotamine tartrate around the corner and hydrolyse like in smith book :
Dissolve 20mg of the alkaloid (previous extraction) in 200ml 1M KOH
in methanol (ie. dissolve 56g KOH pellets in 1L 100% methanol) in a 1L
heavy walled vacuum flask and evaporate the methanol in vacuum at room
temperature. To prevent flask from cooling, thus prolonging the
evaporation time place flask in a pan of water maintained at room
temperature by gently heating or warm water running through. Add 400
ml 8% KOH in water to the residue and boil for one hour .
Cool, acidify with dilute sulfuric acid and
shake in separatory funnel with 1L ether. Discard the upper ether
layer and filter the aqueous suspension of lysergic acid(I) in
vacuum. Wash precipitate with 20ml dilute sulfuric acid. and so and so on...
And I would get a workable result.
Now I have Ergometrine Maleate and I tried Shulgins synth. first:
A solution of 6.7 g KOH in 100 mL H2O, magnetically stirred, was brought to 75 °C, and 10 g ergotamine tartrate (ET) added. The reaction mixture turned yellow as the ergotamine went into solution over the course of 1 h. The stirring was continued for an additional 3 h. The reaction mixture was cooled to about 10 °C with an external ice bath, and acidified to a pH of about 3.0 by the dropwise addition of 2.5 N H2SO4. White solids started to appear early in the neutralization; approximately 60 mL of sulfuric acid was required
When I added 10 Gram of Ergometrine Maleate to the solution which was 75 centigrade, it first turned yello, then reddish, then brown like coffee and smelled like caramel.I let it stirr at 75 for 3 H, then:
I neutralised to a ph of 3.Result: NOTHING, not even after the night in the fridge.
OK, next try:
The classic one, like on top of this page,
I found out, that 10 gram ergometrine maleate does not dissolve in 100 ml 1M KOH Methanol solution, I evaporated
der vacuum anyway and added 200ml 8% KOH
I made the 8% KOH solution by making a saturated KOH in Water solution and then filled 80 ml of this in a 1 liter measuring cylinder and added dest. water till I reached 1 liter, hope this was right, but it did work before...
At around 45 centigrade the solution would turn brown, I put the temp at 90 centigrade for 2 hours, then cool, neutralise, but only recive about 2 g of Lysergic acid.
Then I tried Shulgins synth with higher temp, like reflux, Took samples inbetween, no result. another 10 g gone.
Tried the classic one again , this time boiling under reflux for 1 h 15 min got 1,4 g lsa.
These yields are lousy, what am i doing wrong?
I know that ergometrine maleate takes longer to convert, at least that is what otto snow wrote in his book, and since I take 10 ml samples every half hour I belive he is right.
Where can i find a cool synth for ergometrine maleate? My stock is shrinkin...