反应详情

温度

100 °C

To a RBF were added 5-hydroxy-2-pyridinecarboxylic acid methyl ester (1.2 ml, 9.94 mmol), sodium chlorodifluoroacetate (3.3 g, 21.54 mmol), and cesium carbonate (9.7 g, 29.8 mmol) in DMF (20 ml). The reaction mixture was heated to 100° C. for 3 h. Then it was cooled to RT. The reaction mixture was diluted with water and extracted with EtOAc. The organic extract was washed with water, brine and dried over MgSO4. It was filtered and concentrated. The crude product was purified by flash chromatography eluting with a gradient of 5% to 50% EtOAc in hexane, to provide methyl 5-(difluoromethoxy)picolinate (1.4962 g, 7.37 mmol, 74.1% yield). MS m/z: 204.3 [M+H].

1. temperatureThen it was cooled to RT
2. extractionextracted with EtOAc
3. extractionThe organic extract
4. washwas washed with water, brine
5. dry with materialdried over MgSO4
6. filtrationIt was filtered
7. concentrationconcentrated
8. customThe crude product was purified by flash chromatography
9. washeluting with a gradient of 5% to 50% EtOAc in hexane