反应详情

A solution of acid 18 (0.20 g, 0.65 mmol) in THF (15 mL) was added with DEPC (0.13 mL, 1.3 mol eq) and the mixture was stirred at room temperature for 10 minutes. Then [3-[4-(trifluoromethoxy)phenyl]phenyl]methanamine 23B (0.19 g, 1.1 mol eq) and a catalytic amount of TEA were added, then the reaction mixture was stirred at room temperature overnight. The solvent was removed under reduced pressure, the residue was suspended in EtOAc (45 mL) and washed with water (40 mL) and brine. The separated organic phase was dried over an. Na2SO4 and evaporated under reduced pressure. The residue was purified by flash chromatography (1/1 EtOAc/Petroleum ether) to afford a white solid (0.2 g). Yield=59%, 1HNMR (DMSO, 200 MHz) δ 1.23 (m, 5H), 1.41 (m, 2H), 3.36 (m, 2H), 4.39 (d, 2H, J=6.1), 7.25 (m, 2H), 7.45 (m, 4H), 7.57 (m, 2H), 7.79 (d, 2H, J=7.9), 8.09 (t, 1H). [M+1] 559.31 (C24H22ClF3N2O4S2 requires 559.02).

1. stirringthe reaction mixture was stirred at room temperature overnight
2. customThe solvent was removed under reduced pressure
3. washwashed with water (40 mL) and brine
4. customThe separated organic phase was dried over an
5. customNa2SO4 and evaporated under reduced pressure
6. customThe residue was purified by flash chromatography (1/1 EtOAc/Petroleum ether)