反应详情

Concentrated hydrochloric acid (1 mL) was added dropwise to a mixture of 4-methylthiophenyl hydrazine (2 g, 10.5 mmol) and 4,4-dimethyl-3-oxopentane nitrile (1.44 g, 11.5 mmol) in ethanol (30 mL) and the mixture was heated under reflux for 18 hours. The cooled mixture was then diluted with ethyl acetate, washed with saturated sodium hydrogen carbonate solution, dried over magnesium sulfate and concentrated in vacuo. The residue was purified by column chromatography on silica gel, eluting with dichloromethane:methanol, 100:0 to 97:3 to afford the title compound as a yellow oil that crystallised on standing (2.59 g, 95% yield).

1. temperaturethe mixture was heated
2. temperatureunder reflux for 18 hours
3. washwashed with saturated sodium hydrogen carbonate solution
4. dry with materialdried over magnesium sulfate
5. concentrationconcentrated in vacuo
6. customThe residue was purified by column chromatography on silica gel
7. washeluting with dichloromethane