反应详情

温度

-20 °C

To a cooled (−20° C.) solution of 5-Methylene-2-(4-trifluoromethoxy-phenyl)-tetrahydro-cyclopenta[c]pyrrole-1,3-dione (0.7 g, 2.25 mmol) in EtOH/dichloromethane (15/10 mL) were sequentially added CeCl3. 7H2O (1.0 g, 2.7 mmol) and NaBH4 (0.84 g, 22.5 mmol). The mixture was stirred for 0.5 h at −20° C., then poured into cold water (20 mL) and extracted with dichloromethane (2×15 mL). The solvent was removed by reduced pressure and the residue was purified by silica gel column (petroleum ether/ethyl acetate=5:1) to yield the title compound (0.55 g, 78%). H NMR (300 MHz, CDCl3): δ 7.64-7.60 (m, 2H), 7.25-7.22 (m, 2H), 5.67-5.61 (m, 1H), 5.07 (s, 1H), 4.98 (s, 1H), 3.21-3.09 (m, 2H), 2.81-2.56 (m, 5H); LC-MS: [M+1]+ 314.1.

1. extractionextracted with dichloromethane (2×15 mL)
2. customThe solvent was removed by reduced pressure
3. customthe residue was purified by silica gel column (petroleum ether/ethyl acetate=5:1)