反应详情

To a solution of methyl-L-valinate hydrochloride (168 mg) in dichloromethane (6 mL) was added HOBt (135 mg), 3,5-difluorophenylacetic acid (172 mg), EDCI (191 mg) and DIEA (0.522 mL). The reaction mixture was stirred for 16 h, diluted with dichloromethane (50 mL), washed with 5% hydrochloric acid (10 mL) and 10% potassium carbonate (10 mL). The organic layer after drying over anhydrous magnesium sulfate and concentration under reduced pressure afforded the title compound (272 mg). 1H NMR (300 MHz, CDCl3) δ 0.87 (d, 1.5H, J=7 Hz), 0.89 (d, 1.5H, J=7 Hz), 2.01 (m, 1H), 3.58 (s, 2H), 3.63 (s, 3H), 4.18 (d,d, 1H, J=6 Hz, J=8 Hz), 7.0 (m, 3H), 8.45 (d, 1H, J=8 Hz). MS APCI, m/z=244(M+1). LC/MS: 1.97 min.

1. washwashed with 5% hydrochloric acid (10 mL) and 10% potassium carbonate (10 mL)
2. dry with materialThe organic layer after drying over anhydrous magnesium sulfate and concentration under reduced pressure