Trichloroacetyl chloride → HCID 18449079, compound

Participants

Reaction Steps

To a solution of 10-(4-cyclohexylbenzoyl)-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine of Example 4 (1.85 g) in dichloromethane (50 mL) was added trichloroacetyl chloride (1 g). After stirring overnight at room temperature, the mixture was washed with saturated aqueous sodium bicarbonate, dried over anhydrous sodium sulfate, and filtered through a short column of Magnesol®. After eluting with several additional volumes of dichloromethane, the eluate was combined and refluxed with gradual addition of hexane until crystallization was observed. The title compound (1.5 g) was obtained upon cooling, as colorless crystals, m.p. 172–174° C.

Provenance & Evidence