反应详情

To a stirred solution of tert-butyl 3,5-difluoro-4-formylbenzoate (21 g, 86.7 mmol) in MeOH was portionwise added NaBH4 (3.28 g, 86.7 mmol) at 0° C. After 20 min, the reaction mixture was evaporated in vacuo and the product was extracted with ethyl acetate. The organic layer was washed with brine, dried over MgSO4 and evaporated in vacuo. The residue was purified by flash column chromatography (Hex/EtOAc=4:1) to give tert-butyl 3,5-difluoro-4-(hydroxymethyl)benzoate (20.7 g, 97%) as a white solid.

1. customat 0° C
2. customthe reaction mixture was evaporated in vacuo
3. extractionthe product was extracted with ethyl acetate
4. washThe organic layer was washed with brine
5. dry with materialdried over MgSO4
6. customevaporated in vacuo
7. customThe residue was purified by flash column chromatography (Hex/EtOAc=4:1)