反応 #66162

反応方程式

ethyl pyridin-3-ylacetate

dimethylformamide diethyl acetal

→

Ethyl 3-(dimethylamino)-2-pyridin-3-ylacrylate

反応条件

後処理

1. 1
   温度After cooling
2. 2
   濃縮the mixture is concentrated
3. 3
   その他the residue is initially pre-purified by flash chromatography on silica gel (mobile phase: gradient cyclohexane/ethyl acetate 1:1 ethyl acetate/ethanol 9:1)
4. 4
   その他The product obtained in this manner
5. 5
   workup.DISTILLATIONis then subjected to fine purification by distillation under reduced pressure (1 mbar, bath temperature 200° C.)

実験手順

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 initially pre-purified by flash chromatography on silica gel (mobile phase: gradient cyclohexane/ethyl acetate 1:1 ethyl acetate/ethanol 9:1). The product obtained in this manner is then subjected to fine purification by distillation under reduced pressure (1 mbar, bath temperature 200° C.).

出典