反应详情

a suspension of lithium aluminum hydride (13.75 g, 365.75 mmol) in anhydrous diethyl ether (500 mL) was added via a powder addition funnel 2,6-dichlorophenylacetic acid (50 g, 243.75 mmol). The resulting reaction mixture was refluxed for 16 hours and then quenched by slow addition of a sodium sulfate saturated aqueous solution (25 mL). The resulting slurry was stirred for 3 hours and then filtered, the insoluble was carefully washed with diethyl ether (2×100 mL). The combined ether filtrates were dried over sodium sulfate and the solvent was evaporated in vacuo to yield 38.6 g (85% yield) of the title compound.

1. customThe resulting reaction mixture
2. temperaturewas refluxed for 16 hours
3. customquenched by slow addition of a sodium sulfate saturated aqueous solution (25 mL)
4. filtrationfiltered
5. washthe insoluble was carefully washed with diethyl ether (2×100 mL)
6. dry with materialThe combined ether filtrates were dried over sodium sulfate
7. customthe solvent was evaporated in vacuo