反应详情

A stirred mixture of 29.3 kg of crude (3β,5α)-3-(benzoyloxy)cholest-8(14)en-15-one (6) (Example 3) in 190 liters of methanol in a 100-gallon glass-lined reactor was treated with 8 5 kg of potassium carbonate, the mixture was heated to gentle reflux and held at reflux for 3 hours. The methanol solution was cooled, then was treated with 130 liters of water and 80 liters of heptane with vigorous stirring. The agitation was stopped and the mixture was chilled to 0° C. to -5° C. for 16 hours The crystalline mass was broken up by agitation and the solid was filtered, washed with 100 liters of methanol at 15° C, then air-dried to yield 21.3 kg of the desired crude product. The crude product was recrystallized as follows: A solution of the crude product, 21.3 kg, in 180 liters of methanol at about 45° C. was filtered through a pad of diatomaceous earth using nitrogen pressure. The filtrate was added to 200 liters of heptane at 45°-50° C. Then the solution was treated by vigorous agitation with 100 liters of water preheated to 60° C. The mixture was agitated for 10 minutes, then cooled to 35° C. over a 3-hour period, followed by standing at 25° C. for 24 hours and finally the mixture was chilled to 3° C.

1. temperaturethe mixture was heated
2. temperatureto gentle reflux
3. temperatureat reflux for 3 hours
4. temperaturethe mixture was chilled to 0° C. to -5° C. for 16 hours The crystalline mass
5. filtrationthe solid was filtered
6. washwashed with 100 liters of methanol at 15° C
7. customair-dried