WillD
Expert
- Joined
- Jul 19, 2021
- Messages
- 716
- Reaction score
- 1,011
- Points
- 93
1. A slurry of 3.15 g d-lysergic acid monohydrate and 7.3 g diethylamine in 150 ml of pure chloroform is heated for reflux.
2. After the lysergic acid is dissolved (a few min) cool the mixture down to where reflux has stopped by removing the heat.
3. Before the mixture cools any further 2ml of phosphorous oxychloride is added at such a rate as to give reflux (about 2 min).
4. In addition, reflux for 4-5 min further, until an amber-colored solution results.
5. Cool to room temp and wash the mixture with 200ml of 1M ammonium hydroxide.
6. The chloroform solution was dried with MgSO4 (this would have to be after separation), filtered, and concentrated by evaporation in vacuum under a temp of 38 *C (at no time let the temp go over 40 *C).
7. Dissolved the residue in a minimum amount of methanol and acidify with a freshly prepared solution of 20% maleic acid in methanol (not aqueous) to precipitate the LSD in its maleate form.
8. Filter the fluffy white needles, was with cold methanol and air dry to get 2.2 g of LSD that requires no further purification.
2. After the lysergic acid is dissolved (a few min) cool the mixture down to where reflux has stopped by removing the heat.
3. Before the mixture cools any further 2ml of phosphorous oxychloride is added at such a rate as to give reflux (about 2 min).
4. In addition, reflux for 4-5 min further, until an amber-colored solution results.
5. Cool to room temp and wash the mixture with 200ml of 1M ammonium hydroxide.
6. The chloroform solution was dried with MgSO4 (this would have to be after separation), filtered, and concentrated by evaporation in vacuum under a temp of 38 *C (at no time let the temp go over 40 *C).
7. Dissolved the residue in a minimum amount of methanol and acidify with a freshly prepared solution of 20% maleic acid in methanol (not aqueous) to precipitate the LSD in its maleate form.
8. Filter the fluffy white needles, was with cold methanol and air dry to get 2.2 g of LSD that requires no further purification.
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