反应详情

To a solution of 4-bromo-3,5-dihydroxybenzoic acid (13.89 g, 59.6 mmol) in methanol (50 mL) was added H2SO4 (concentrated, 1 mL). The reaction mixture was heated to reflux overnight. The mixture was quenched with H2O (500 mL) and extracted with 10% MeOH in CH2Cl2 (5×500 mL), dried over MgSO4 and concentrated in vacuo to give a white solid (14.8 g, 100% yield). 1H NMR (400 MHz, DMSO-d6) δ 10.47 (s, 2 H) 7.00 (s, 2 H) 3.80 (s, 3 H); LCMS for C8H7BrO4 m/z 249.10 (M+H)+.

1. temperatureThe reaction mixture was heated
2. temperatureto reflux overnight
3. customThe mixture was quenched with H2O (500 mL)
4. extractionextracted with 10% MeOH in CH2Cl2 (5×500 mL)
5. dry with materialdried over MgSO4
6. concentrationconcentrated in vacuo