反应详情

NCS (1.44 g, 10.8 mmol) and benzoyl peroxide (238 mg, 0.98 mmol) were added to a stirred solution of 2-chloro-3-cyano-6-methyl-pyridine (750 mg, 4.92 mmol) in benzene (35 mL) and the mixture was heated to reflux. After 4 h, the mixture was cooled and filtered. The filtrate was diluted with ethyl acetate and was washed with sodium metabisulfite solution, water and brine, dried (Na2SO4) and evaporated in vacuo. The residue was purified by chromatography on silica (chloroform) to give the title compound:

1. temperaturethe mixture was heated to reflux
2. temperaturethe mixture was cooled
3. filtrationfiltered
4. additionThe filtrate was diluted with ethyl acetate
5. washwas washed with sodium metabisulfite solution, water and brine
6. dry with materialdried (Na2SO4)
7. customevaporated in vacuo
8. customThe residue was purified by chromatography on silica (chloroform)