反应详情

温度

60 °C

A solution of trimethyl phosphonoacetate (4.0 g) in toluene (10 ml) was added to a mixture of sodium hydride (63%, 880 mg) in toluene (45 ml) with stirring and cooling and then heated at 60° C. for 20 minutes. To the mixture 2-phenylpyrazolo[1,5-a]pyridine-3-carbaldehyde (2.0 g) was added and heated at 60° C. for 8 hours. A saturated sodium bicarbonate solution (30 ml) was added to the reaction mixture and extracted with ethyl acetate (30 ml, 2 times). The extract was washed with brine (30 ml), dried over magnesium sulfate and evaporated in vacuo. The residue was recyrstallized from a mixture of ethyl acetate and isopropyl alcohol to give crystals of methyl 3-(2-phenylpyrazolo[1,5-a]pyridin-3-yl)acrylate (trans isomer) (1.34 g).

1. temperaturecooling
2. temperatureheated at 60° C. for 8 hours
3. extractionextracted with ethyl acetate (30 ml, 2 times)
4. washThe extract was washed with brine (30 ml)
5. dry with materialdried over magnesium sulfate
6. customevaporated in vacuo
7. additionThe residue was recyrstallized from a mixture of ethyl acetate and isopropyl alcohol