Oxalyl chloride → HCID 10167445, compound

Participants

Reaction Steps

To a stirred solution of 10-(4-cyclohexyl-benzoyl)-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine of Example 4 (1.0 g) in dichloromethane (20 mL) was added oxalyl chloride (0.34 g). The reaction mixture was allowed to stir at room temperature for three hours, and then 4-(1-piperidino) piperidine (0.91 g) was added. After stirring overnight at room temperature, the mixture was washed with water and saturated aqueous sodium bicarbonate and dried over anhydrous sodium sulfate. The solution was filtered through a short column of Magnesol® and the eluate refluxed with the slow addition of hexane to provide the title compound as pale pink crystals (0.43 g), m.p. 190–195° C.

Provenance & Evidence