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Trichloroacetyl chloride → 2-(Chloromethyl)-3,4-dimethylpyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trichloroacetyl chloride | HCID 6420 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 2,3,4-Trimethyl-1-oxidopyridin-1-ium | HCID 18735286 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 2-(Chloromethyl)-3,4-dimethylpyridine | HCID 19996500 | — |
反応手順
A solution of 13.3 g of 2,3,4-trimethylpyridine N-oxide in 130 ml of abs. chloroform is boiled at reflux under argon and treated through the condenser with 33.2 ml of trichloroacetyl chloride. After 18 hours the reaction mixture is poured on to ice, whereupon 10% sodium bicarbonate solution is added, the mixture is extracted with methylene chloride and the methylene chloride solution is dried and concentrated. The thus-obtained crude product is chromatographed on silica gel (solvent: methylene chloride/ether [5:1]). The 2-chloromethyl-3,4-dimethylpyridine obtained is processed directly.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04766133 |
| 出典データセット | uspto-grants-1988_08 |
| ORD ID | ord-b6036994e5e34e789174b720aa134be6 |
| 出典メモ | uspto-grants-1988_08 |