反应详情

2,3-difluorobenzoic acid (9.47 g, 59.90 mmol) and H2SO4 (0.3 mL) in methanol (100 mL) were heated for 3 days in a 70° C. oil bath. The reaction was cooled to RT, then the solvent was removed under vacuum at 35° C. The crude residue was transferred to a separatory funnel with ether, washed with saturated sodium bicarbonate solution (2×50 mL), brine, dried (MgSO4), filtered and concentrated under vacuum. The residue was redissolved in CH2Cl2, dried (MgSO4), filtered and concentrated under vacuum to yield 8.66 grams of methyl 2,3-difluorobenzoate as a clear liquid.

1. customthe solvent was removed under vacuum at 35° C
2. customThe crude residue was transferred to a separatory funnel with ether
3. washwashed with saturated sodium bicarbonate solution (2×50 mL), brine
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated under vacuum
7. dissolutionThe residue was redissolved in CH2Cl2
8. dry with materialdried (MgSO4)
9. filtrationfiltered
10. concentrationconcentrated under vacuum