反应详情

To a solution of 4-chloro-o-tolyloxyacetic acid chloride of step A (17.4 mmol) in dichloromethane (25 mL) was added a solution of 10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine (17.4 mmol) and triethylamine (19.14 mmol) in dichloromethane (25 mL) in a rapid dropwise fashion. The mixture was stirred for one hour at room temperature. The reaction mixture was washed with 0.1 N hydrochloric acid (2×) and water (1×), dried over anhydrous sodium sulfate and evaporated. The product was isolated by crystallization from hot ethyl acetate/t-butyl methyl ether (2/1), m.p. 166-167° C. MS [(+)ESI, m/z]: 367 [M+H]+ Anal. Calcd for C21H19CIN2O2: C, 68.76; H, 5.22; N, 7.64. Found: C, 68.53; H, 5.18; N, 7.53.

1. washThe reaction mixture was washed with 0.1 N hydrochloric acid (2×) and water (1×)
2. dry with materialdried over anhydrous sodium sulfate
3. customevaporated
4. customThe product was isolated by crystallization from hot ethyl acetate/t-butyl methyl ether (2/1), m.p. 166-167° C