反应详情

Add lithium aluminum hydride (5.18 mL, 5.18 mmol, 1M solution in THF) to a solution of methyl difluorophenylethanoate (0.964 g, 5.18 mmol, prepared by following the procedure described in J. Org. Chem. 1995, 60, 5174-5179) in anhydrous THF (10 mL) at 0° C. Stir the mixture at room temperature for 45 min. Cool to 0° C. and quench with EtOAc and then water. Separate the organic phase and extract twice the aqueous phase with EtOAc. Dry the combined organic extracts over Na2SO4, filter and concentrate in vacuo to provide the desired intermediate (0.8 g, 98%) that was used without any further purification.

1. customprepared
2. customat 0° C
3. temperatureCool to 0° C.
4. customquench with EtOAc
5. customSeparate the organic phase
6. extractionextract twice the aqueous phase with EtOAc
7. dry with materialDry the combined organic extracts over Na2SO4
8. filtrationfilter
9. concentrationconcentrate in vacuo