反应详情

温度

100 °C

NaCN (4 g, 82 mmol) was added to a solution of 3-bromo-6-fluoro-2-methyl-pyridine (4 g, 21 mmol) in DMSO (100 mL) The mixture was stirred for 2 h at 100° C., poured into H2O (100 mL) and extracted with ethyl acetate (2×100 mL). The organic layers were dried over Na2SO4, concentrated and purified by flash column chromatography (silica gel, 10 g, eluting with 10% ethyl acetate in petroleum ether) to give the title compound (0.6 g, 15%) as white solid; MS (EI): m/e=197.0 [1\4+H]+.

1. extractionextracted with ethyl acetate (2×100 mL)
2. dry with materialThe organic layers were dried over Na2SO4
3. concentrationconcentrated
4. custompurified by flash column chromatography (silica gel, 10 g, eluting with 10% ethyl acetate in petroleum ether)