反应详情

A mixture of the 9,10-dihydro-4H-3a, 5,9-triaza-benzo[f]azulene of Step D (4.67 mmol), 4-cyclohexylbenzoyl chloride (4.90 mmol) and triethylamine (5.1 mmol) in 1,2-dichloroethane was refluxed for three days under nitrogen. The solvent was removed in vacuo and the residue chromatographed on silica gel eluting with a solvent gradient from 5 to 20% of ethyl acetate in hexane to provide the title compound as a tan solid (0.684 g), m.p. 150–152° C.

1. temperaturewas refluxed for three days under nitrogen
2. customThe solvent was removed in vacuo
3. customthe residue chromatographed on silica gel eluting with a solvent gradient from 5 to 20% of ethyl acetate in hexane