反应详情

To a stirred solution of 0.362 g of 2-methoxybenzoyl chloride 5 ml of methylene chloride is added 0.346 g of triethylamine at 0° C. After stirring for 3 minutes, 0.500 g of 10,11-dihydro-10-(4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine is added and stirring continued for 18 hours at room temperature. The reaction mixture is diluted with 45 ml of methylene chloride and washed with water, 2N citric acid, 1M NaHCO3, and brine. The reaction mixture is dried with Na2SO4, filtered through hydrous magnesium silicate and evaporated in vacuo to give a solid which is purified by crystallization from ethyl acetate to give 0.430 g of the desired product as a crystalline solid, m.p. 185°-188° C.

1. stirringstirring
2. waitcontinued for 18 hours at room temperature
3. washwashed with water, 2N citric acid, 1M NaHCO3, and brine
4. dry with materialThe reaction mixture is dried with Na2SO4
5. filtrationfiltered through hydrous magnesium silicate
6. customevaporated in vacuo
7. customto give a solid which
8. customis purified by crystallization from ethyl acetate