反应详情

A solution of 0.55 g (4.54 mmol) of 2-methylpyridine-5-carboxaldehyde in toluene was added dropwise into a cool suspension of 1.12 g (5 mmol) of ethyl diethylphosphonoacetate and 0.12 g (5 mmol) of NaH in toluene and the resulting solution was allowed to react at 65° C. for 30 min. After cooling, the mixture was filtered through SUPERCEL™ (wash SUPERCEL™ with ether) and concentrated in vacuo to yield 0.71 g (87.6%) of ethyl β-(2-methylpyridin-3-yl)acrylate (cis/trans mixture), which was further purified through a silica plug (hexane/ethyl acetate, 1:1).

1. customto react at 65° C. for 30 min
2. temperatureAfter cooling
3. filtrationthe mixture was filtered through SUPERCEL™ (wash SUPERCEL™ with ether)
4. concentrationconcentrated in vacuo