반응 #595374

반응 방정식

methyl 4-bromo-2,5-difluorobenzoate

NaOMe

→

title compound

methyl 4-bromo-5-fluoro-2-methoxybenzoate

용매

DMF

반응 조건

후처리

1. 1
   workup.WAITat rt for 30 min
2. 2
   기타was then brought back to 0° C.
3. 3
   기타quenched with EtOAc and 1M HCl
4. 4
   기타The organic layer was separated
5. 5
   추출the aqueous phase was extracted with EtOAc
6. 6
   건조dried over Na2SO4
7. 7
   농축concentrated
8. 8
   기타purified by flash chromatography (Pentane/EtOAc=9:1)

실험 절차

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

출처