化工社化工社 化学情報印刷レポート · 研究参考用
Dimethylformamide diethylacetal → 3-(Dimethylamino)-2-pyridin-3-yl-acrylic acid ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide diethylacetal | HCID 70913 | — |
| 反応物 | Ethyl 3-pyridylacetate | HCID 96490 | — |
| 生成物 | 3-(Dimethylamino)-2-pyridin-3-yl-acrylic acid ethyl ester | HCID 68704864 | — |
反応手順
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.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08524699B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-2fab76d5241947dead68d408eaf254c6 |
| 出典メモ | uspto-grants-2013_09 |