HRID1186049

反应详情

EQUATION

反应方程式

HRID 1186049 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The title compound can be synthesized from hydrocortisone acetate according to the procedure disclosed in EP 0097328. 405 g (1 mol) of hydrocortisone acetate is added to a mixture of 2 liters of N,N-dimethylformamide and 350 ml of pyridine, and with stifling at room temperature, 260 g of methanesulfonyl chloride is added. The reaction mixture is heated, maintained at 80 to 85° c. for 1 hour, and then cooled to room temperature. Methanol (7 liters) is added. The precipitated crystals are separated by filtration, washed with methanol and water, and dried under reduced pressure to give the title compound.

WORKUP

后处理

  1. customwith stifling at room temperature
  2. temperatureThe reaction mixture is heated
  3. temperaturemaintained at 80 to 85° c
  4. customThe precipitated crystals are separated by filtration
  5. washwashed with methanol and water
  6. customdried under reduced pressure