WillD
Expert
- Joined
- Jul 19, 2021
- Messages
- 809
- Reaction score
- 1,113
- Points
- 93
1. Dissolve 175 g KOH in 1750 ml of water in a flask of 5 liters volume equipped with a reflux condenser and gas inlet tube. If a stirring device is not required, it should be removed and the open neck stoppered.
2. Heat the mixture to 80 *C, and add 500 g of ergotamine tartrate. Hold the temp at 80 *C for 2 hours.
3. Pour the mixture into a 5 gallon polyethylene bucket (made from the same material as a plastic) filed with about 6 liters of ice. Put the bucket in a cooling mixture to cool below 10 *C.
4. Neutralize the mixture by adding cold dilute sulfuric acid to a congo red end point (pH 4.2). Lysergic acid and potassium sulphate will be seen to precipitate.
5. Let stand for 2-3 hours, possible.
6. Break up the filter cake and put in a 2 liter beaker.
7. Make a solution from 150 ml of liquid ammonia and 2.5 liters of very cold dry denaturated ethanol and add to the reaction mixture.
8. Stir for 1 hour and filter. Keep the filtrate and treat the filter cake to the ammonia ethanol mixture as above.
9. This second extract is filtered, and the cake is washed with 250 ml of the ammoniacal ethanol mixture.
10. Combine the filtrates, and evaporate to total dryness with a strong vacuum and gently heating. Do not heat at too high of a temp.
11. Scrape the product from the vacuum vessel and put into a mortar.
12. Mix 113 ml of methanol with 38 ml of water, and rinse the product. The slurry in the mortar is ground up well and filtered.
13. Wash the filter cake and dry 80-85 *C under a high vacuum to get about 65-75 g of cream-white to grey-white powder. This is lysergic acid monohydrate.
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