反应详情

To a stirred solution of 1-(4-methylpyridin-2-yl)propan-1-one (0.9 g) in chloroform (5 ml) was added a solution of sulfuryl chloride (0.533 ml) in chloroform (5 ml) dropwise. The resultant mixture was refluxed for 2 hours and evaporated under reduced pressure. The pH was adjusted to 8.5 with a saturated aqueous sodium hydrogencarbonate solution, and the mixture was extracted with ethyl acetate twice. The combined organic layer was washed with brine, dried over magnesium sulfate and evaporated under reduced pressure. The residue was purified by column chromatography (silica gel 25 g, n-hexane:dichloromethane=1:1) to give 2-chloro-1-(4-methylpyridin-2-yl)propan-1-one (0.71 g).

1. customevaporated under reduced pressure
2. extractionthe mixture was extracted with ethyl acetate twice
3. washThe combined organic layer was washed with brine
4. dry with materialdried over magnesium sulfate
5. customevaporated under reduced pressure
6. customThe residue was purified by column chromatography (silica gel 25 g, n-hexane:dichloromethane=1:1)