反应详情

温度

110 °C

Under an atmosphere of argon, a mixture of 4-(4-bromophenyl)-1-(3-(difluoromethyl)-phenyl)-3,4,7,8-tetrahydroquinazoline-2,5(1H,6H)-dione (intermediate 33, 75 mg, 0.168 mmol), zinc cyanide (34 mg, 0.290 mmol) and tetrakis(triphenylphosphine)-palladium(0) (20 mg, 17 μmol) in N,N-dimethylformamide (1 mL) is heated at 110° C. for 2 h and cooled to room temperature. Water is added and the mixture is extracted twice with dichloromethane. The combined organic layers are dried over Na2SO4 and concentrated under reduced pressure. The residue is purified by flash chromatography on silica (gradient cyclohexane/ethyl acetate 100:0 to 0:100). Yield: 30 mg; ESI mass spectrum [M+H]+=394; Retention time HPLC: 0.53 min (X012_S01).

1. temperaturecooled to room temperature
2. extractionthe mixture is extracted twice with dichloromethane
3. dry with materialThe combined organic layers are dried over Na2SO4
4. concentrationconcentrated under reduced pressure
5. customThe residue is purified by flash chromatography on silica (gradient cyclohexane/ethyl acetate 100:0 to 0:100)
6. custom0.53 min (X012_S01)