反应详情

1.0 g of 3-(3-thienyl)benzaldehyde, 0.5 g of cyanoacetic acid, 15 mg of ammonium acetate and 1 ml of pyridine were dissolved in 1.5 ml of xylene, and the mixture was refluxed for 5.5 hours. The solvent was evaporated, and the residue was dissolved in a mixture of ethyl ether and water, then the resulting solution was acidified with diluted hydrochloric acid. The organic layer separated was worked up in a customary manner, and the product purified by medium-pressure liquid chromatography [silica gel column, hexane/ethyl acetate=7/1→5/1] to give 0.4 g of (E)-3-(3-thienyl)cinnamonitrile as a white powder.

1. temperaturethe mixture was refluxed for 5.5 hours
2. customThe solvent was evaporated
3. dissolutionthe residue was dissolved in a mixture of ethyl ether and water
4. customThe organic layer separated
5. customthe product purified by medium-pressure liquid chromatography [silica gel column, hexane/ethyl acetate=7/1→5/1]