HRID17846

反应详情

EQUATION

反应方程式

HRID 17846 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

To a solution of 7-chloro-4-cyclopropylmethyl-4H-1,2,4-benzothiadiazine 1,1-dioxide (0.7 g) in isopropanol (50 mL) there is added sodium borohydride (0.2 g) and the mixture is heated at 50° C. for 5 minutes. The reaction mixture is evaporated under reduced pressure and the residue is taken up in water (30 mL). The pH of the medium is adjusted to 5-6 by addition of 6N hydrochloric acid and the suspension is extracted three times with chloroform (30 mL). The organic phases are collected, dried over anhydrous MgSO4 and filtered. The filtrate is evaporated under reduced pressure and the residue is taken up in methanol (5 mL). Water (50 mL) is added to the methanolic solution and the precipitate which appears is collected by filtration, washed with water and dried.

WORKUP

后处理

  1. customThe reaction mixture is evaporated under reduced pressure
  2. additionThe pH of the medium is adjusted to 5-6 by addition of 6N hydrochloric acid
  3. extractionthe suspension is extracted three times with chloroform (30 mL)
  4. customThe organic phases are collected
  5. dry with materialdried over anhydrous MgSO4
  6. filtrationfiltered
  7. customThe filtrate is evaporated under reduced pressure
  8. additionWater (50 mL) is added to the methanolic solution
  9. filtrationthe precipitate which appears is collected by filtration
  10. washwashed with water
  11. customdried