反应详情

A mixture of 5.365 g (20 mmol) of 4-(3-n1trophenyl)-3-pyridyl-3-butene-2-one, 15.417 g (100 mmol) of 2-cyanoethyl 3-aminocrotonate, 5.451 g (40 mmol) of zinc chloride, and 10 g of Molecular Shieves 4A was added to 1,4-dioxane. This reaction mixture was refluxed with application of heat in an inert atmosphere for 5 hours. The reaction mixture was then cooled to room temperature and neutralized with a saturated aqueous solution of sodium hydrogencarbonate, followed by extraction with chloroform. The solvents contained in the extract were distilled off and the residue was chromatographed on a silica gel column, whereby the captioned compound was obtained. The yield was 7.94 g (87%).

1. temperatureThis reaction mixture was refluxed with application
2. temperatureof heat in an inert atmosphere for 5 hours
3. extractionfollowed by extraction with chloroform
4. distillationwere distilled off
5. customthe residue was chromatographed on a silica gel column, whereby the captioned compound
6. customwas obtained