反应详情

Sodium hydride (60% in mineral oil, 1.06 g, 26.5 mmol) is added at room temperature in portions to a mixture of 3-(3-(trifluoromethyl)phenylamino)cyclopent-2-enone (4.31 g, 17.9 mmol) and 2-methyltetrahydrofuran. After 20 min tert-butyl(4-cyanophenyl)(phenyl-sulfonyl)methylcarbamate (10.0 g, 24.2 mmol based on 90% purity) is added, and the mixture is stirred at room temperature for 1 h. Water is added and the phases are separated. The organic layer is washed with water and concentrated under reduced pressure, and the residue is recrystallized from tert-butyl methyl ether. Yield: 6.92 g. ESI mass spectrum: [M+H]+=472; Retention time HPLC: 0.76 min (X012_S01).

1. customthe phases are separated
2. washThe organic layer is washed with water
3. concentrationconcentrated under reduced pressure
4. customthe residue is recrystallized from tert-butyl methyl ether
5. custom0.76 min (X012_S01)