反应详情

A solution of 10-[(2-methoxy-2′-methyl-1,1′-biphenyl-4-yl)carbonyl]-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine of Step E (21 mmol) and triethylamine (43 mmol) in anhydrous dichloromethane (45 mL) was cooled in an ice bath. To the stirred solution was added, dropwise, trichloroacetyl chloride (65 mmol). The mixture was allowed to stir at ambient temperature for 72 hours. The solution was washed with 0.1 N hydrochloric acid and brine and dried over anhydrous sodium sulfate. Evaporation gave a green foam. This was crystallized by heating in ethyl acetate and chloroform to give 10.2 g of the title compound as a white powder (85%), m.p. 221-222° C.

1. additionTo the stirred solution was added
2. washThe solution was washed with 0.1 N hydrochloric acid and brine
3. dry with materialdried over anhydrous sodium sulfate
4. customEvaporation
5. customgave a green foam
6. customThis was crystallized
7. temperatureby heating in ethyl acetate