反应详情

To a solution of 3-chloro-4-methylbenzoic acid (20 g, 117 mmol) in MeOH (200 mL) was added dropwise thionyl chloride (25.6 mL, 352 mmol) at 0° C. with stirring. The mixture was stirred at room temperature for 5 days. The reaction was concentrated. The residue was dissolved in EA (500 mL), washed with 10% Na2CO3 (250 mL×2), water (250 mL) and brine (250 mL), dried over Na2SO4, filtered and concentrated to afford product as a yellow solid (20.8 g, 96%).

1. stirringThe mixture was stirred at room temperature for 5 days
2. concentrationThe reaction was concentrated
3. dissolutionThe residue was dissolved in EA (500 mL)
4. washwashed with 10% Na2CO3 (250 mL×2), water (250 mL) and brine (250 mL)
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated