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Dimethylformamide → 1-[6-(Chloromethyl)pyridin-2-yl]ethanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | 1-(6-(Hydroxymethyl)pyridin-2-yl)ethanone | HCID 10329447 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 1-[6-(Chloromethyl)pyridin-2-yl]ethanone | HCID 11819445 | — |
反応手順
Phosphorus oxychloride (7.8 ml) was dropwise added to a mixture of 2-acetyl-6-hydroxymethylpyridine (10.0 g) and N,N-dimethylformamide (15.4 ml) in ethyl acetate (100 ml) under ice-cooling with stirring and the mixture was stirred at the same temperature for 3 hours. The reaction mixture was added to water and adjusted to pH 7.5 with potassium carbonate. The separated organic layer was washed with brine, dried over magnesium sulfate and evaporated to give 2-acetyl-6-chloromethylpyridine (10.85 g) as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05364871 |
| 出典データセット | uspto-grants-1994_11 |
| ORD ID | ord-b49227bd87f64e7ba28744faa948c3c7 |
| 出典メモ | uspto-grants-1994_11 |