反应详情

温度

5 °C

To a solution of NHMe(OMe).HCl (20.3 g, 0.21 mol) in THF (110 mL), H2O (40 mL) and TEA (26.3 g, 0.22 mol) was added 2,3,5-trifluorophenylacetic acid (42, 24.7 g, 0.13 mol) and CDI (24.3 g, 0.15 mol) at 0-10° C. The reaction mixture was stirred at 0-10° C. for 5 h. After HPLC showed that the reaction was complete, the mixture was filtered through celite and the filtrate was partitioned with water and EtOAc. The organic solution was dried over Na2SO4 and concentrated. The crude residual was further purified by flash chromatography on silica gel (5-10% EtOAc/PE) to give 43 (24.0 g, 80% yield). 1H NMR (CDCl3, 400 MHz): δ 6.76-6.72 (m, 2H), 3.72 (m, 2H), 3.66 (d, 3H), 3.15 (d, 3H); MS (ESI) m/e [M+H]+: 234.07.

1. filtrationthe mixture was filtered through celite
2. customthe filtrate was partitioned with water and EtOAc
3. dry with materialThe organic solution was dried over Na2SO4
4. concentrationconcentrated
5. customThe crude residual was further purified by flash chromatography on silica gel (5-10% EtOAc/PE)