反应详情

37.4 g (226 mmol) of ethyl pyridin-3-ylacetate in 100 g (679 mmol) of dimethylformamide diethyl acetal are heated at 100° C. overnight. After cooling, the mixture is concentrated and the residue is prepurified by flash chromatography on silica gel (mobile phase: gradient cyclohexane/ethyl acetate 1:1→ethyl acetate/ethanol 9:1). The resulting product is subjected to fine purification by vacuum distillation (1 mbar, 200° C. bath temperature).

1. temperatureAfter cooling
2. concentrationthe mixture is concentrated
3. distillationThe resulting product is subjected to fine purification by vacuum distillation (1 mbar, 200° C. bath temperature)