反应详情

0.45 g (1.22 mmol) of ethyl (2Z, 4E)-6-(2,5-dimethoxyphenyl)-6-oxo-3-phenylhexa-2,4-dienoate, 20 ml of ethanol, 0.206 g (2.44 mmol) of sodium bicarbonate and 20 ml of water are mixed together and refluxed for three hours. After evaporating off the solvents, the residue is poured into water, acidified with normal hydrochloric acid solution and extracted with dichloromethane. The organic phase is dried (Na2SO4), the solvent is evaporated off and the pasty product obtained is purified by flash chromatography (20/80 heptane/ethyl acetate) (yellow solid; diisopropyl ether; m.p.: 165° C.; 170 mg) and recrystallized (10/6 hexane/ethyl acetate) (0.3 g of yellow solid; 22%).

1. temperaturerefluxed for three hours
2. customAfter evaporating off the solvents
3. additionthe residue is poured into water
4. extractionextracted with dichloromethane
5. dry with materialThe organic phase is dried (Na2SO4)
6. customthe solvent is evaporated off
7. customthe pasty product obtained
8. customis purified by flash chromatography (20/80 heptane/ethyl acetate) (yellow solid; diisopropyl ether; m.p.: 165° C.; 170 mg)
9. customrecrystallized (10/6 hexane/ethyl acetate) (0.3 g of yellow solid; 22%)