Purification of LSD-25 Tartrate
The material obtained by any of these preparations may contain both lysergic
acid and iso-lysergic
acid amides. Method 1 contains mostly iso-lysergic diethylamide and must be converted prior to separation. For this material, go to Step II first.
Step I. Use darkroom and follow with a long wave UV
Reagants:
Iso-Lysergic Acid Diethylamine
Benzene
Chloroform
Methanol
Tartaric Acid
Equipment:
Chromatography Column
Vacuum Distillation Apparatus
UV Light source
1. The material is dissolved in a 3:1 mixture of benzene and chloroform.
2. Pack the chromatography column with a slurry of basic alumina in benzene so that a 1 inch column is six inches long.
3. Drain the solvent to the top of the alumina column and carefully add an aliquot of the LSD-solvent solution containing 50 ml of solvent and 1 g LSD.
4. Run this through the column, following the fastest moving fluorescent band.
5. After it has been collected, strip the remaining material from the column by washing with MeOH.
6. Use the UV light sparingly to prevent excessive damage to the compounds.
7. Evaporate the second fraction in vacuo and set aside for Step II.
8. The fraction containing the pure LSD is concentrated in vacuo and the syrup will crystallise slowly.
9. This material may be converted to the tartrate by titration with tartaric
acid and the LSD tartrate conveniently crystallised. MP 190-196 C.
Step II. Use Red light
Reagants:
Methanol
4M KOH Solution (alcoholised)
Dilute HCl
Ammonium Hydroxide solution
Chloroform
Indicator
Equipment:
Pipette
Vacuum Distillation Apparatus
Chromatography Column
1. Dissolve the residue derived from the methanol stripping of the column in a minimum amount of alcohol.
2. Add twice that volume of 4 N alcoholic KOH solution and allow the mixture to stand at room temperature for several hours.
3. Neutralise with dilute HCl, make slightly basic with NH4OH and extract with chloroform or ethylene dichloride as in preparations #1 or #2.
4. Evaporate in vacuo and chromatograph as in the previous step.
Lysergic
acid compounds are unstable to heat, light and oxygen. In any form it helps to add ascorbic
acid as an anti- oxidant, keeping the container tightly closed, light-tight with aluminum foil, and in a refrigerator.