反应详情

To 1-bromo-2,4-dimethylbenzene (1.85 g) were added 1-BOC-1,4]diazepane (2 g), palladium (II) acetate (0.115 g), rac-2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (0.31 g), sodium tert-butoxide (1.34 g) and toluene (35 mL), and the mixture was refluxed for 9 hr. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, and the solvent was evaporated. The residue was purified by column chromatography (chloroform:methanol) to give 4-(2,4-dimethylphenyl)-[1,4]diazepane-1-carboxylic acid tert-butyl ester (2.16 g). To 4-(2,4-dimethylphenyl)-[1,4]diazepane-1-carboxylic acid tert-butyl ester (2.16 g) were added 4N hydrogen chloride/ethyl acetate (6.9 mL) and chloroform (17 mL), and the mixture was stirred at room temperature overnight. The solvent was evaporated to give the title compound (1.74 g).

1. customThe solvent was evaporated