反应详情

温度

0 °C

To a solution of methyl 4-bromo-2,5-difluorobenzoate (i-7c) (0.5 g, 2 mmol) in DMF (5 mL) at 0° C. was added NaOMe (25% in MeOH, 0.45 mL, 2 mmol). The reaction mixture was stirred at 0° C. for 10 min and then at rt for 30 min. The mixture was then brought back to 0° C. and quenched with EtOAc and 1M HCl. The organic layer was separated, and the aqueous phase was extracted with EtOAc, dried over Na2SO4, concentrated and purified by flash chromatography (Pentane/EtOAc=9:1) to give the title compound. LCMS (ESI) calc'd for C9H8BrFO3 [M+H]+: 263. found: 263

1. waitat rt for 30 min
2. customwas then brought back to 0° C.
3. customquenched with EtOAc and 1M HCl
4. customThe organic layer was separated
5. extractionthe aqueous phase was extracted with EtOAc
6. dry with materialdried over Na2SO4
7. concentrationconcentrated
8. custompurified by flash chromatography (Pentane/EtOAc=9:1)