反应详情

温度

71 °C

Solid LiOH (5.04 g, 210 mmol) was added to a stirred solution of phenylmethyl 5-bromo-2-[(phenylmethyl)oxy]benzoate (may be prepared as described in Description 4, method C, 15 g, 37.8 mmol) in THF (150 ml) and water (50.0 ml) at 20° C. The reaction mixture was stirred at 71° C. overnight. After cooling to room temperature, the reaction mixture was diluted with ethyl acetate (200 ml). 10% aqueous HCl was added to the mixture to adjust the pH to 2. The organic phase was isolated, washed with brine, dried over Na2SO4 and concentrated to give a white solid. The crude product was purified by silica gel chromatography eluting with hexane:ethyl acetate (3:1) to yield the title compound. 6.1 g.

1. temperatureAfter cooling to room temperature
2. customThe organic phase was isolated
3. washwashed with brine
4. dry with materialdried over Na2SO4
5. concentrationconcentrated
6. customto give a white solid
7. customThe crude product was purified by silica gel chromatography
8. washeluting with hexane:ethyl acetate (3:1)