HRID867523
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
7.3 g (25 mmol) of 7-chloro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylic acid are suspended in 50 ml of N,N-dimethylformamide, whereupon the suspension is treated with 5.67 g (34 mmol) of 1,1'-carbonyldiimazole and the mixture is stirred at room temperature for a further 0.75 hour and subsequently at 60° for 2 hours. The mixture is then poured into 100 ml of water, the product is filtered off under suction after 1 hour, rinsed with water and dried at 80° in a high vacuum. There is obtained 1-[[7-chloro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepin-3-yl]carbonyl]imidazole of decomposition point 242°-244°.
WORKUP
后处理
- additionis treated with 5.67 g (34 mmol) of 1,1'-carbonyldiimazole and the mixture
- filtrationthe product is filtered off under suction after 1 hour
- washrinsed with water
- customdried at 80° in a high vacuum