反应详情

A solution of 1-bromo-4-(chloro(isocyanato)methyl)benzene (240 mg, 0.974 mmol) in dichloromethane (2 mL) is added dropwise to a solution of 3-(3-(difluoromethyl)phenyl-amino)cyclopent-2-enone (intermediate 5, 217 mg, 0.974 mmol) in dichloromethane (2 mL) and the reaction mixture is heated at reflux for 2 h. Water is added, and the phases are extracted twice with dichloromethane. The combined organic layers are concentrated and the residue is purified by flash chromatography on silica (gradient cyclohexane/ethyl acetate 4:1 to ethyl acetate). Yield: 159 mg; ESI mass spectrum: [(79Br)-M+H]+=433, [(81Br)-M+H]+=435; Retention time HPLC: 0.56 min (X012_S01).

1. temperaturethe reaction mixture is heated
2. temperatureat reflux for 2 h
3. extractionthe phases are extracted twice with dichloromethane
4. concentrationThe combined organic layers are concentrated
5. customthe residue is purified by flash chromatography on silica (gradient cyclohexane/ethyl acetate 4:1 to ethyl acetate)
6. custom0.56 min (X012_S01)