反应详情

温度

100 °C

A mixture of isonicotinaldehyde (25 g), ethyl(triphenylphosphoranylidene)acetate (82 g) and toluene (300 ml) is stirred for 3 hours at 100° C. After cooling, the crystals that precipitated are removed by filtration, and the filtrate is concentrated in vacuo. The residue is dissolved in a mixture of ethyl acetate and petroleum ether (1:1, 400 ml), and the resulting solution is extracted with 5% hydrochloric acid (500 ml). The aqueous layer is extracted with ethyl acetate (50 ml) and neutralized with potassium carbonate. After cooling, the resulting crystals are collected by filtration and dried to give ethyl 3-(4-pyridyl)acrylate (34 g) as colorless prisms, mp 64°-66° C.

1. temperatureAfter cooling
2. customthe crystals that precipitated
3. customare removed by filtration
4. concentrationthe filtrate is concentrated in vacuo
5. dissolutionThe residue is dissolved in a mixture of ethyl acetate and petroleum ether (1:1, 400 ml)
6. extractionthe resulting solution is extracted with 5% hydrochloric acid (500 ml)
7. extractionThe aqueous layer is extracted with ethyl acetate (50 ml)
8. temperatureAfter cooling
9. filtrationthe resulting crystals are collected by filtration
10. customdried