反应详情

温度

60 °C

To 2-chloro-4,5-difluoro-benzoic acid (118, 14.0 g, 0.0727 mol) in methanol (100 mL) was added sulfuric acid (concentrated, 98%, 2.00 mL, 0.0375 mol). The reaction was stirred at 60° C. for 48 hours. The reaction was poured into water and extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated and purified by silica gel column chromatography eluting with 20% ethyl acetate in hexane to give a colorless oil (119, 13.0 g, 86.6%).

1. extractionextracted with ethyl acetate
2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
3. filtrationfiltered
4. concentrationThe filtrate was concentrated
5. custompurified by silica gel column chromatography
6. washeluting with 20% ethyl acetate in hexane
7. customto give a colorless oil (119, 13.0 g, 86.6%)