O-Xylene → HCID 10280053, compound

Participants

Reaction Steps

A mixture of 10-(4-cyclohexyl-benzoyl)-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine of Example 4 (1.85 g), dry xylene (25 mL) and 4-tert-butylbenzoylchloride (1.97 g) was refluxed overnight. The reaction mixture was poured into water, 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 combined eluate was refluxed with the gradual addition of hexane until crystallization was noted. Cooling and trituration provided the desired title product (0.18 g) as off-white crystals, m.p. 143–145° C.

Provenance & Evidence