HRID356653

反应详情

EQUATION

反应方程式

HRID 356653 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

0.1 g of the compound obtained in Example 37 in 3 ml of ethanol was treated with 0.014 g of sodium borohydride. The reaction mixture was stirred at 80° C. for 1 hour. Thereafter, the ethanol was distilled off and the residue was partitioned between chloroform and 1 N HCl. The organic phase was washed with water and dried, the solvent was evaporated and the residue was chromatographed over silica gel with chloroform-methanol. After recrystallization from dichloromethane-ethanol there was obtained 0.072 g of 5-isopropyl-pyridine-2-sulphonic acid 5-(2-chloro-5-methoxy-phenoxy)-6-hydroxymethyl-2-morpholin-4-yl-pyrimidin-4-ylamide. M.p. 105° C.

WORKUP

后处理

  1. distillationThereafter, the ethanol was distilled off
  2. customthe residue was partitioned between chloroform and 1 N HCl
  3. washThe organic phase was washed with water
  4. customdried
  5. customthe solvent was evaporated
  6. customthe residue was chromatographed over silica gel with chloroform-methanol
  7. customAfter recrystallization from dichloromethane-ethanol there