Lysergic acid recrystallization

[Zarder]

What is the best solvent and method for LA recrystallization? I’ve read in Otto Snows book that water can be used. I know that LA is almost completely insoluble in water at RT.
Other than that what solvent can be used?
Also I feel like I’d struggle to hot filter it without it crashing out so will just a recrystallization in the beaker work to purify the LA?

 

[G.Patton]

p. 3114

The acid could be purified by dissolving it in dilute ammonium hydroxide, treating with decolorizing carbon, and reprecipitating with carbon dioxide, m.p. 242-243° dec.; a mixture m.p. with dl-lysergic acid made from natural d-lysergic acid was likewise 242-243° dec.

https://pubs.acs.org/doi/pdf/10.1021/ja01594a039

Sci-Hub | The Total Synthesis of Lysergic Acid. Journal of the American Chemical Society, 78(13), 3087–3114 | 10.1021/ja01594a039

(+)-Lysergic acid total synthesis

Introduction Lysergic acid, the basic fragment derived from the ergot alkaloids, has been synthesized in a fourteen sequence beginning with 3-beta-carboxyethylindole. The starting material was converted to the intermediate 1-benzoyl-5-keto-1,2,2a-3,4,5-hexahydrobenz-[cd]-indole (3), containing...

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[Zarder]

p. 3114

https://pubs.acs.org/doi/pdf/10.1021/ja01594a039

Sci-Hub | The Total Synthesis of Lysergic Acid. Journal of the American Chemical Society, 78(13), 3087–3114 | 10.1021/ja01594a039

(+)-Lysergic acid total synthesis

Introduction Lysergic acid, the basic fragment derived from the ergot alkaloids, has been synthesized in a fourteen sequence beginning with 3-beta-carboxyethylindole. The starting material was converted to the intermediate 1-benzoyl-5-keto-1,2,2a-3,4,5-hexahydrobenz-[cd]-indole (3), containing...

bbgate.com

G.Patton

Writeup: Lsd synthesis from ergocristine using PyBOP

100ml of 10% KOH solution was added to an rbf under inert atmosphere (Ar). This was let to stir and brought up to 75-80C. 5g of ergocristine was added to the flask and the rxn mixture turned yellow as the reaction progressed. The rxn was let to stir for 3 hours and became a homogeneous yellow...

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So somewhat similar to this procedure?

“
The solids obtained were washed with et2o, suspended in nh4oh/etoh and insolubles removed by filtration. This was repeated three times.
The colourless filtrate was stripped under high vacuum using a rotovap, dissolved in 1% nh4oh and acidified with 40% sulfuric acid. The precipitated solids were filtered, washed with et2o until free of colour
and dried under vacuum until constant mass. 2g of lysergic acid hydrate was obtained. This was heated under high vacuum until the mass decreased to the stoichiometric anhydrous form.”

 

[G.Patton]

So somewhat similar to this procedure?

ZarderWhat is a source of this manual?

 

[Zarder]

What is a source of this manual?

G.PattonIt’s a forum post

Writeup: Lsd synthesis from ergocristine using PyBOP

100ml of 10% KOH solution was added to an rbf under inert atmosphere (Ar). This was let to stir and brought up to 75-80C. 5g of ergocristine was added to the flask and the rxn mixture turned yellow as the reaction progressed. The rxn was let to stir for 3 hours and became a homogeneous yellow...

bbgate.com