反应详情

A solution of 10,11-dihydro-5-methyl-dibenzo[b,e][1,4]diazepine of Step C (0.42 g) in dichloromethane (10 mL) containing N,N-diisopropylethyl amine (0.29 g) was treated with 4-cyclohexylbenzoyl chloride (0.50 g). After stirring overnight at room temperature, the reaction mixture was washed with water and saturated aqueous sodium bicarbonate, then dried over anhydrous sodium sulfate. The solution was filtered through a short column of Magnesol® which was eluted with several additional volumes of dichloromethane. Evaporation of all volatiles gave a glassy residue which was triturated with anhydrous diethyl ether to provide the title compound as an off-white crystalline solid (0.66 g), m.p. 111–112° C.

1. washthe reaction mixture was washed with water and saturated aqueous sodium bicarbonate
2. dry with materialdried over anhydrous sodium sulfate
3. filtrationThe solution was filtered through a short column of Magnesol® which
4. washwas eluted with several additional volumes of dichloromethane
5. customEvaporation of all volatiles
6. customgave a glassy residue which
7. customwas triturated with anhydrous diethyl ether