反应详情

A mixture of thioisonicotinamide (2.76 g) and ethyl 2-chloroacetoacetate (3.6 g) in ethanol (30 ml) was heated for 20 hours under reflux and the solvent was evaporated. To the residue was added saturated sodium hydrogen carbonate solution, and the solution was extracted with ethyl acetate. The extract was washed with water, dried and concentrated. The residue was subjected to silica gel chromatography, and eluted with hexane-ethyl acetate (2:1) to give the title compound as crystals (2.0 g, 40.3%).

1. temperaturewas heated for 20 hours
2. temperatureunder reflux
3. customthe solvent was evaporated
4. additionTo the residue was added saturated sodium hydrogen carbonate solution
5. extractionthe solution was extracted with ethyl acetate
6. washThe extract was washed with water
7. customdried
8. concentrationconcentrated
9. washeluted with hexane-ethyl acetate (2:1)