反应详情

温度

30 °C

A solution of (R)-ethyl 4-(4-((4′-chlorobiphenyl-2-yl)(diethoxyphosphoryloxy)methyl)piperidin-1-yl)benzoate (INTERMEDIATE 119, 500 mg, 0.85 mmol) in THF (10 ml) and MeOH (2.5 ml), at room temperature, was treated with a solution of lithium hydroxide (102 mg, 4.27 mmol) in water (2.5 ml). The reaction was heated to 30° C. overnight and subsequently warmed to 40° C. for about 5 hours. The mixture was allowed to cool to room temperature whereupon the volatiles were removed under reduced pressure. The concentrate was diluted with 30 ml of water, acidified with a few drops of 6N HCl to provide a white precipitate. The precipitate was collected by vacuum filtration to give the title compound (410 mg, yield: 86%).

1. temperaturesubsequently warmed to 40° C. for about 5 hours
2. temperatureto cool to room temperature whereupon the volatiles
3. customwere removed under reduced pressure
4. additionThe concentrate was diluted with 30 ml of water
5. customto provide a white precipitate
6. filtrationThe precipitate was collected by vacuum filtration