反应详情

温度

0 °C

To a suspension of methyl 3,4-dihydroxybenzoate (5.0 g) in diethyl ether (300 mL) stirred at 0° C. was added sulfuryl chloride (3.7 mL) dropwise. The reaction mixture was stirred at 0° C. for 16 h. The solvent was removed in vacuo. The residue was washed with hot chloroform (2×150 mL) to afford methyl 3-chloro-4,5-dihydroxybenzoate (D68) (1.9 g) as a white solid. δH (DMSO-d6, 400 MHz): 3.78 (3H, s), 7.33 (1H, d), 7.37 (1H, d), 10.11 (2H, br s). MS (ES): C8H7ClO4 requires 202. found 203.0 (M+H+).

1. stirringThe reaction mixture was stirred at 0° C. for 16 h
2. customThe solvent was removed in vacuo
3. washThe residue was washed with hot chloroform (2×150 mL)