反应详情

To a stirred solution of 0.406 g of 4-chloro-2-methoxybenzoyl chloride in 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. An additional 0.406 g of 4-chloro-2-methoxybenzoyl chloride and 0.346 g of triethylamine is added and stirring is continued for 2 hours. 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 and evaporated in vacuo to give a residue which is purified by flash chromatography using 1:1 ethyl acetate-hexane to give a solid which is crystallized from ethyl acetate to give 0.320 g of the desired product as a white crystals, m.p. 222°-224 ° C.

1. stirringstirring
2. waitcontinued for 18 hours at room temperature
3. stirringstirring
4. waitis continued for 2 hours
5. washwashed with water, 2N citric acid, 1M NaHCO3, and brine
6. dry with materialThe reaction mixture is dried with Na2SO4
7. filtrationfiltered
8. customevaporated in vacuo
9. customto give a residue which
10. customis purified by flash chromatography
11. customto give a solid which
12. customis crystallized from ethyl acetate