反应详情

To a stirred solution of benzenesulfonamide (40 mg, 0.26 mmol), sodium hydride (11 mg, 0.49 mmol) and N,N-dimethylformamide (2 mL) was added dropwise a solution of phenyl 2-[4-(3,5-dimethyl-4-phenyl-1H-pyrazol-1-yl)phenyl]ethylcarbamate (step 1, 100 mg, 0.24 mmol) in N,N-dimethylformamide (2 mL) at room temperature. After 2 h, the mixture was poured into ice-water and extracted with dichloromethane. The organic layer was dried over MgSO4 and evaporated in vacuo. The residue was purified by TLC with dichloromethane/methanol (10:1) to give 84 mg (73%) of the title compound as white solids: 1H-NMR (CDCl3) δ 7.89 (2H, d, J=8.2 Hz), 7.64-7.21 (12H, m), 6.33 (1H, br.s), 3.51-3.44 (2H, m), 2.84 (2H, t, J=6.8 Hz), 2.33 (3H, s), 2.24 (3H, s).

1. extractionextracted with dichloromethane
2. dry with materialThe organic layer was dried over MgSO4
3. customevaporated in vacuo
4. customThe residue was purified by TLC with dichloromethane/methanol (10:1)