反应 #2308001

反应方程式

4-chlorobutanoylchloride

triethylamine

hydrocortisone

→

Hydrocortisone (4-chloro)butanoate

收率 53.0%

溶剂

CHCl3

反应条件

后处理

1. 1
   干燥dried over P2O5
2. 2
   workup.ADDITIONThe solution was treated with water
3. 3
   其他the organic phase was separated
4. 4
   干燥dried (Na2SO4)
5. 5
   其他to give a white solid with a 53% yield by weight, which
6. 6
   其他a melting point (m.p.) of 155° C.

实验过程

4 portions of 4-chlorobutanoylchloride (0.32 ml×4) and triethylamine (0.3 g×4) were added in 24 hours to a solution of hydrocortisone (1 g) in CHCl3 dried over P2O5, and stirred for 3 days. The solution was treated with water, the organic phase was separated, dried (Na2SO4) and deprived of the solvent at reduced pressure. The crude residue was ground with hexane and CH2Cl2 to give a white solid with a 53% yield by weight, which had a melting point (m.p.) of 155° C.

来源