反应详情

To 2-chloro-4,5-difluoro-benzoic acid methyl ester (119, 5.70 g, 0.0276 mol) in tetrahydrofuran (120.0 mL), 1.00 M of lithium tetrahydroaluminate in tetrahydrofuran (30.0 mL) was added slowly under an atmosphere of nitrogen. The reaction was stirred at room temperature for 4 hours, followed by adding sodium sulfate decahydrate. After 30 minutes, the reaction mixture was filtered, concentrated and purified with silica gel column chromatography eluting with 8% methanol in dichloromethane to give a white solid (120, 4.20 g, 85.2%).

1. waitAfter 30 minutes
2. filtrationthe reaction mixture was filtered
3. concentrationconcentrated
4. custompurified with silica gel column chromatography
5. washeluting with 8% methanol in dichloromethane
6. customto give a white solid (120, 4.20 g, 85.2%)