反应详情

A solution of 10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine (0.37 g) and diisopropylethylamine (0.61 g) in dichloromethane (25 ml) was cooled to 0° C. and a solution of 6-(1-methyl-1H-pyrazol-4-yl)pyridine-3-carbonyl chloride in dichloromethane (25 ml) was added portionwise. After 18 hours at room temperature, the reaction mixture was washed with water and a saturated aqueous sodium bicarbonate solution. The dichloromethane solution was dried over anhydrous sodium sulfate and filtered through a short column of hydrous sodium magnesium silicate and further eluted with several volumes of dichloromethane. The combined organic phase was concentrated on a hot plate with the gradual addition of hexane until crystallization occurred. After cooling, the crystals were collected by filtration to yield the title compound (0.31 g), m.p. 173-175° C.; MS, m/z: 370.3 (M+H)+.

1. washthe reaction mixture was washed with water
2. dry with materialThe dichloromethane solution was dried over anhydrous sodium sulfate
3. filtrationfiltered through a short column of hydrous sodium magnesium silicate
4. washfurther eluted with several volumes of dichloromethane
5. concentrationThe combined organic phase was concentrated on a hot plate with the gradual addition of hexane until crystallization
6. temperatureAfter cooling
7. filtrationthe crystals were collected by filtration