反应详情

To the solution of 4-(trifluoromethyl)phenylacetonitrile (2560.9 mg; 13.83 mmol; 1.06 eq.) in ethanol (50 mL), 21% sodium ethoxide (5.70 ml; 15.27 mmol; 1.17 eq.) in ethanol was added dropwise at RT. After stirred for 30 min, a solution of 1-boc-4-piperidone (2600.00 mg; 13.05 mmol; 1.00 eq.) in ethanol (10 mL) was added slowly. The reaction mixture was stirred at room temperature for 4 h. The reaction was quenched with 50 mL of saturated aqueous NH4Cl and concentrated to half volume. The aqueous solution was extracted with ether three times. The combined organic extracts were washed with brine, dried and then concentrated to give the crude product, which was purified by Biotage chromatography with EtOAc/Hexane (5-30%) to yield the desired product as light yellow solid (3200.00 mg, yield 66.9%).

1. stirringThe reaction mixture was stirred at room temperature for 4 h
2. customThe reaction was quenched with 50 mL of saturated aqueous NH4Cl
3. concentrationconcentrated to half volume
4. extractionThe aqueous solution was extracted with ether three times
5. washThe combined organic extracts were washed with brine
6. customdried
7. concentrationconcentrated
8. customto give the crude product, which
9. customwas purified by Biotage chromatography with EtOAc/Hexane (5-30%)