反应详情

温度

0 °C

To a solution of 5-chloro-2-methoxy-benzoic acid methyl ester (20 g, 9.97 mmol) in THF (100 mL) at 0° C. was added dropwise a solution of lithium aluminum hydride (210 mL, 210 mmol, 1M soln. in THF). The solution was then warmed to reflux for 2 hours. The reaction was cooled to 0° C. and carefully quenched by the addition of cold water. The mixture was filtered through celite and the filter cake was washed with diethyl ether. The filtrate was washed with saturated aqueous sodium hydrogen carbonate then dried over magnesium sulfate. Concentration in vacuo gave the title compound (17.2 g).

1. temperatureThe solution was then warmed
2. temperatureto reflux for 2 hours
3. customcarefully quenched by the addition of cold water
4. filtrationThe mixture was filtered through celite
5. washthe filter cake was washed with diethyl ether
6. washThe filtrate was washed with saturated aqueous sodium hydrogen carbonate
7. dry with materialthen dried over magnesium sulfate
8. concentrationConcentration in vacuo