反应详情

温度

70 °C

H2SO4 (0.5 mL, 9.3 mmol) was added to a suspension of 2-bromo-5-methoxy-4-methylbenzoic acid (4.07 g, 16.6 mmol) in MeOH (40 mL) and the resulting rxn mixture was heated to 70° C. overnight. The rxn mixture was cooled to 0° C. and basified with 1M aq. NaOH (10 mL) to pH 11. The rxn mixture was extracted with DCM and the combined org. layers were dried (MgSO4), filtered and concentrated in vacuo to yield methyl 2-bromo-5-methoxy-4-methylbenzoate as a yellow solid that was used as such in the next step without purification. LC-MS A: tR=0.90 min, [M+H]+=258.91.

1. temperatureThe rxn mixture was cooled to 0° C.
2. extractionThe rxn mixture was extracted with DCM
3. dry with materiallayers were dried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated in vacuo