HRID223190
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
A mixture of 5.7 g (0.018 mol) of 3,4-dihydro-6-iodo-4-methyl-2H-1,4-benzodiazepine-2,5(1H)-dione, 2.4 g (0.026 mol) of copper (I) cyanide and 60 ml of dimethylformamide is heated to 50° for 45 minutes. After cooling, the mixture is diluted with water and extracted several times with chloroform/isopropanol (4:1). The combined organic extracts are dried over magnesium sulphate and evaporated. The yellow-brown crude product is recrystallized from methanol, there being obtained 2,3,4,5-tetrahydro-4-methyl-2,5-dioxo-1H-1,4-benzodiazepine-6-carbonitrile of melting point 253-256.
WORKUP
后处理
- temperatureis heated to 50° for 45 minutes
- temperatureAfter cooling
- extractionextracted several times with chloroform/isopropanol (4:1)
- dry with materialThe combined organic extracts are dried over magnesium sulphate
- customevaporated
- customThe yellow-brown crude product is recrystallized from methanol, there