反应详情

温度

26 °C

A stirred mixture of 28.4 kg (3β,5α,15α)-14,15-epoxycholest-7-en-3-ol benzoate (3) (Example 2) in 280 liters of acetone, under nitrogen, in a 200gallon reactor, at 22° C. was treated with 100 ml of 70% perchloric acid. The mild exothermic reaction raised the reaction mixture temperature to 26° C. in about a 5 minute period The mixture was cooled to 21° C. and an additional 180 ml of 70% perchloric acid was added. The reaction mixture temperature was kept at 22±1° C. and the mixture was stirred for 3 hours to complete the reaction. The mixture was cooled and treated with 140 liters of water at 19° C. for 30 minutes, then stirred 20 minutes more. The solid was collected by filtration, washed with a large quantity of water and dried in vacuo at 40°-60° C. to give 29.3 kg of the desired crude product (6).

1. customThe mild exothermic reaction
2. temperaturewas cooled to 21° C.
3. customwas kept at 22±1° C.
4. customthe reaction
5. temperatureThe mixture was cooled
6. stirringstirred 20 minutes more
7. filtrationThe solid was collected by filtration
8. washwashed with a large quantity of water
9. customdried in vacuo at 40°-60° C.