A suspension of 3.15 g d-lysergic acid hydrate and 7.1 g of diethylamine in 150 mL CHCl3 was brought to reflux with stirring. With the external heating removed, there was added 3.4 g POCl3 over the course of 2 min...
If I have done the math correctly, 3.15 g of d-lysergic acid hydrate is 3.15/300.332*1000 = 10.5 mmol, 7.1 g of diethylamine is 7.1/72.129*1000 = 98.4 mmol, and 3.4 g of phosphorus oxychloride is 3.4/153.332*1000 = 22.2 mmol. I believe that there should be 2 moles of POCl3 for every mole of d-lysergic acid hydrate--one mole to react with the hydrate part and one mole to chlorinate the lysergic acid. Is there a reason that he used a slight excess? Why did he use so much diethylamine?
Oxygen69
Post 465132 (https://www.thevespiary.org/talk/index.php?topic=13102.msg46513200#msg46513200)
(Rhodium: "Garbrecht's Classic LSD Synthesis", Tryptamine Chemistry)Why did he use so much diethylamine?
The excess diethylamine is used to neutralize the HCl that would be formed otherwise.
(https://www.thevespiary.org/rhodium/Rhodium/hive/hiveboard/picproxie_docs/000463737-file_e2yo.jpg)