Acetic Acid → HCID 13187315, compound

Participants

Reaction Steps

To a refluxing 100 ml of propanol were simultaneously added, over a period of 20 minutes, in small portions 5 g of sodium and a solution of 5 g of holamine in 5 ml of propanol while continuing reflux. After 1 hour and 25 minutes, the temperature was returned to ambient, the mixture chilled and acidified with acetic acid to pH 6. The pH raised to pH 8 with potassium carbonate and the mixture was diluted with 500 ml of water, partially evaporated, 300 ml of water were added and the mixture was allowed to crystallize for 24 hours in the refrigerator. The filtered crystals were washed in water and dissolved in 10 ml of methylene chloride to which was added 50 ml of ethyl acetate and 30 ml of isopropyl ether. The methylene chloride was evaporated and the product allowed to crystallize during 16 hours in the refrigerator. 3 g of 3α-amino pregn-5-ene- 20-ol was obtained melting at 160°.

Provenance & Evidence