HRID1199315

反应详情

EQUATION

反应方程式

HRID 1199315 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A 24.55 kg amount of (3β,5α)-cholesta-7,14-dien-3-ol benzoate (2) (prepared in the manner described in Example 1) and 6.41 g of sodium bicarbonate were suspended under nitrogen with good agitation in 240 liters of t-butyl methyl ether in a 200-gallon reactor and chilled to 0° C. A solution of 13.0 kg of m-chloroperbenzoic acid in 100 liters of t-butyl methyl ether at about 20° C. was added to the steroid-bicarbonate suspension over a 10 minute period. A mild exothermic reaction which raised the reaction mixture temperature to 10° C. was noted. The mixture was stirred for 2 hours then 150 liters of water were added. The mixture was stirred an additional hour and agitation was halted to allow separation of the phases. The lower aqueous layer was drained off and the remaining organic phase was treated with 50 liters of water, agitated vigorously, and then the aqueous portion was drained off. The product was filtered at about 10° C., washed with three 10 liter portions of methanol and air-dried to yield 19.1 k9 of (3) batch-A.

WORKUP

后处理

  1. customA mild exothermic reaction which
  2. temperatureraised the reaction mixture temperature to 10° C.
  3. stirringThe mixture was stirred an additional hour
  4. customseparation of the phases
  5. additionthe remaining organic phase was treated with 50 liters of water
  6. stirringagitated vigorously
  7. filtrationThe product was filtered at about 10° C.
  8. washwashed with three 10 liter portions of methanol
  9. customair-dried