反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe reaction mixture is evaporated under reduced pressure
- additionThe pH of the medium is adjusted to 5-6 by addition of 6N hydrochloric acid
- extractionthe suspension is extracted three times with chloroform (30 mL)
- customThe organic phases are collected
- dry with materialdried over anhydrous MgSO4
- filtrationfiltered
- customThe filtrate is evaporated under reduced pressure
- additionWater (50 mL) is added to the methanolic solution
- filtrationthe precipitate which appears is collected by filtration
- washwashed with water
- customdried