反应详情

To 1,3-difluoro-2-methylbenzene (5.00 g, 39.0 mmol), chlorosulfuric acid (10.5 mL, 158 mmol) was added with cooling on ice, and the mixture was stirred at room temperature for 5 hours. To the reaction solution, water (100 mL) was added with cooling on ice, followed by extraction with dichloromethane (100 mL). The thus obtained organic layer was dried over anhydrous sodium sulfate. After vacuum concentration, the residue was purified with silica gel chromatography to yield the title compound (8.65 g, 98%) as a colorless amorphous solid.

1. temperaturewith cooling on ice
2. temperaturewith cooling on ice
3. extractionfollowed by extraction with dichloromethane (100 mL)
4. dry with materialThe thus obtained organic layer was dried over anhydrous sodium sulfate
5. concentrationAfter vacuum concentration
6. customthe residue was purified with silica gel chromatography