反应详情

温度

80 °C

A mixture of 4-bromo-3-chlorosulfonyl-benzoic acid (6.90 g, 23.04 mmol, 1.00 Eq) in SOCl2 (27.41 g, 230.40 mmol, 10.00 Eq) was stirred at 80° C. for 3 hr. Then the solvent was evaporated. The residue was diluted in TOLUENE (50 mL), and MeOH (959.66 mg, 29.95 mmol, 1.30 Eq) was added, the formed mixture was stirred at 110° C. for 2 hr. Solid was formed, and the solvent was evaporated, the solid was washed with PE, and filtered to afford product methyl 4-bromo-3-chlorosulfonyl-benzoate (7.22 g, 23.03 mmol, 99.94% yield) as white solid.

1. customThen the solvent was evaporated
2. additionThe residue was diluted in TOLUENE (50 mL)
3. stirringthe formed mixture was stirred at 110° C. for 2 hr
4. customSolid was formed
5. customthe solvent was evaporated
6. washthe solid was washed with PE
7. filtrationfiltered