反应详情

温度

20 °C

Under a nitrogen atmosphere, drop-wise add a solution of (6S)-4-benzyl-6-(4-fluorophenyl) morpholin-3-one (625 g, 2.19 mol) in THF (22 L) to lithium aluminum hydride in THF (1M in THF, 5.0 L, 5 mol) while maintaining the temperature at 20° C. Heat the mixture to 70° C. and stir for 1.5 h. Cool the mixture to 0° C. and add H2O (200 mL) to quench the reaction, followed by aqueous NaOH (4 M, 1.25 L), then add more H2O (600 mL). Stir the resulting mixture for 30 min; filter; and rinse the solid with EtOAc (10 L). Collect the filtrate and concentrate it under reduced pressure to provide the title compound (561 g, 94%). MS (m/z): 272 (M+1).

1. temperatureHeat the mixture to 70° C.
2. temperatureCool the mixture to 0° C.
3. customto quench
4. customthe reaction
5. stirringStir the resulting mixture for 30 min
6. filtrationfilter
7. washand rinse the solid with EtOAc (10 L)
8. customCollect the filtrate
9. concentrationconcentrate it under reduced pressure