HRID867532
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
19 g (60 mmol) of (S)-8-chloro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxamide are suspended in 110 ml of N,N-dimethylformamide, whereupon the suspension is treated with 17 ml (116 mmol) of N,N-dimethylacetamide dimethyl acetal and the mixture is stirred at 115° for 2.5 hours. The mixture is then cooled to 0°, the product is filtered off under suction, rinsed with N,N-dimethylformamide and diethyl ether and dried at 80° in a high vacuum. There is obtained (S)-8-chloro-N-[1-(dimethylamino)ethylidene]-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxamide of decomposition point 289°-291°.
WORKUP
后处理
- temperatureThe mixture is then cooled to 0°
- filtrationthe product is filtered off under suction
- washrinsed with N,N-dimethylformamide and diethyl ether
- customdried at 80° in a high vacuum