HRID1764512
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
PROCEDURE
实验过程
To a suspension of 2.8 parts of 7-chloro-2-hydrazino 5-phenyl-3H-1,4-benzodiazepine in 40 parts by volume of formamide is added 1 part by volume of concentrated sulfuric acid. The resulting solution is left standing for 6 hours and then warmed on a boiling water bath for 30 minutes. The solution is diluted with water, neutralized with sodium bicarbonate and extracted with chloroform. The chloroform extract is washed with water and dried over anhydrous sodium sulfate, followed by evaporation of the solvent. The residue is recrystallized from ethyl acetate to give 8-chloro-6-phenyl-4H-s-triazolo [4,3-a][1,4] benzodiazepine as colorless flakes. Melting point: 226° C to 227° C.
WORKUP
后处理
- waitThe resulting solution is left
- temperaturewarmed on a boiling water bath for 30 minutes
- extractionextracted with chloroform
- extractionThe chloroform extract
- washis washed with water
- dry with materialdried over anhydrous sodium sulfate
- customfollowed by evaporation of the solvent
- customThe residue is recrystallized from ethyl acetate