反应详情

温度

20 °C

Ethyl 3-(3,5-bis(trifluoromethyl)phenyl)-3-cyanopropanoate (1.2 g, 1.0 eq.) was dissolved in MeOH (48 mL). Dichlorocobalt hexahydrate (1.68 g, 2.0 eq.) was added and the reaction mixture was cooled to 20° C. NaBH4 (1.98 g, 15 eq.) was added portion wise by maintaining temperature below 30° C. After completion of addition, this reaction mixture was stirred for 18 h at 25° C. The reaction mixture was concentrated under reduced pressure and the residue was partitioned between ethyl acetate (25 mL) and water (25 mL). The reaction mixture was filtered through Celite™ and the organic layer was separated, dried over Na2SO4, filtered, and concentrated under reduced pressure to afford 0.65 g of crude product, which after trituration with petroleum ether gave 0.5 g of 4-(3,5-bis(trifluoromethyl)phenyl)pyrrolidin-2-one (Yield 47.61%).

1. temperatureby maintaining temperature below 30° C
2. additionAfter completion of addition
3. concentrationThe reaction mixture was concentrated under reduced pressure
4. customthe residue was partitioned between ethyl acetate (25 mL) and water (25 mL)
5. filtrationThe reaction mixture was filtered through Celite™
6. customthe organic layer was separated
7. dry with materialdried over Na2SO4
8. filtrationfiltered
9. concentrationconcentrated under reduced pressure
10. customto afford 0.65 g of crude product, which after trituration with petroleum ether