反应详情

An ethereal solution of methyl magnesium bromide (3 mol/l) (17.6 ml) was added dropwise to a solution of 6-(acetylaminomethyl)-2-pyridinecarbonitrile (3.70 g) in tetrahydrofuran (60 ml) at 5° to 10° C. with stirring. After the mixture was stirred for two hours at the same temperature, cold water (15 ml) was dropped to the mixture under ice-cooling and evaporated in vacuo. The residue was mixed with water and extracted with a mixture of ethyl acetate and tetrahydrofuran. The extract was dried over magnesium sulfate and evaporated in vacuo. The residue was purified by silica gel column chromatography by eluting with a mixture of ethyl acetate and methanol (50:1) to give 2-acetyl-6-(acetylaminomethyl)pyridine (2.70 g).

1. additionwas dropped to the mixture under ice-
2. temperaturecooling
3. customevaporated in vacuo
4. additionThe residue was mixed with water
5. extractionextracted with a mixture of ethyl acetate and tetrahydrofuran
6. dry with materialThe extract was dried over magnesium sulfate
7. customevaporated in vacuo
8. customThe residue was purified by silica gel column chromatography
9. washby eluting with a mixture of ethyl acetate and methanol (50:1)