Author Topic: Sandoz Ltd. LSD synthesis (1946)  (Read 1335 times)

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pHarmacist

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Sandoz Ltd. LSD synthesis (1946)
« on: March 15, 2003, 03:02:00 PM »
Abstract: The diethylamide of d-lysergic acid is prepared by subjecting to the action of diethylamine the azides of d- or dl-lysergic acid or of d- or dl-isolysergic acid or mixtures of these azides, followed by a separation of the required d-lysergic acid diethylamide from the reaction product which also contains d-iso-lysergic acid by chromatographic adsorption or by fractional crystallisation. In examples (1) d-isolysergic acid is treated with sodium nitrite to form the azide which is then reacted with diethylamine in ether solution. The product consisting of a mixture of the diethylamides of d-lysergic and d-isolysergic acids is separated by chromatographic adsorption. The iso - compound is treated with an acid or an alkali to convert it to an equilibrium mixture of the diethylamides of d-lysergic and d-isolysergic acids which may be again treated as before. The d-lysergic acid diethylamide on treatment with d-tartaric acid in methanol yields the neutral tartrate; (2) as in example (1) with slightly varying experimental conditions; (3) rac-isolysergic acid hydrazide is converted into the azide as in example (1) and then reacted with diethylamine to form a mixture of the rac-diethylamides of isolysergic acid and lysergic acids. This mixture is separated by chromatographic adsorption. From the rac-diethylamide of lysergic acid the diethylamide of d-lysergic acid can be obtained by means of the neutral tartrate. Specification 480,822 is referred to.

Patent GB579484


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Preparation of hydrazide of lysergic acid:

Abstract: The hydrazide of lysergic acid, a component of the molecule of several of the alkaloids of ergot and having the formula C16H16O2N2, is prepared by treating its derivatives, i.e. its amides, esters and those of its derivatives found naturally in the ergot-alkaloids, with hydrazine. The reaction is effected by treatment with hydrazine hydrate under reflux or under pressure and may be conducted in an inert atmosphere. Examples describe preparation of lysergic acid hydrazide from (1) lysergic acid methyl-ester; (2) ergotamine; (3) ergotinine; (4) a mixture of ergotamine and ergotaminine; (5) a crude product obtained from the mother liquors of ergotamine extraction.

Patent GB463936


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MeNH2

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Hi all Bees its been a while ( 4 years or so)
« Reply #1 on: March 17, 2003, 02:35:00 AM »
Sound intrusting but i'd like to know more, whats the yeild ect.. thats about the easyest synth on lsd i'v seen, and i'v seen alot! And had a dream or 2:)
    
8)

pHarmacist

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Are you kidding?
« Reply #2 on: March 17, 2003, 02:42:00 AM »
Are you kidding man? This must be _one_ of the most tedious ways to make "acid" from lysergic acid. I posted it for the "historical purposes" only.

For an easy acid synth see:

Post 412547

(pHarmacist: "Synthesis of LSD from Lysergic Acid", Tryptamine Chemistry)



MeNH2

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I wasnt beeing clear
« Reply #3 on: March 19, 2003, 07:06:00 AM »
sorry i was not being clear. i was not talking about the hole synth, just the part of reacting the azide with Diethylamine in ether.no u are right about the synth as a hole.