反应详情

To a stirred solution of 0.362 g of 2-ethoxybenzoyl 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 72 hours at room temperature. The reaction mixture is diluted with 45 ml of methylene chloride and washed with water, 2N citric acid, NaHCO3, and brine. The reaction mixture is dried with Na2SO4, filtered and evaporated in vacuo to give a solid which is purified by flash chromatography using 1:1 ethyl acetate-hexane to give 0.890 g of solid which is crystallized from ethyl acetate to give 0.540 g of the desired product as a white solid, m.p. 160°-176° C.

1. stirringstirring
2. waitcontinued for 72 hours at room temperature
3. washwashed with water, 2N citric acid, NaHCO3, and brine
4. dry with materialThe reaction mixture is dried with Na2SO4
5. filtrationfiltered
6. customevaporated in vacuo
7. customto give a solid which
8. customis purified by flash chromatography