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Sulfuryl chloride → 2-Chloro-1-(4-methylpyridin-2-yl)propan-1-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuryl chloride | HCID 24648 | — |
| 反応物 | 1-(4-Methylpyridin-2-yl)propan-1-one | HCID 18630984 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 2-Chloro-1-(4-methylpyridin-2-yl)propan-1-one | HCID 18667484 | — |
反応手順
To a stirred solution of 1-(4-methylpyridin-2-yl)propan-1-one (0.9 g) in chloroform (5 ml) was added a solution of sulfuryl chloride (0.533 ml) in chloroform (5 ml) dropwise. The resultant mixture was refluxed for 2 hours and evaporated under reduced pressure. The pH was adjusted to 8.5 with a saturated aqueous sodium hydrogencarbonate solution, and the mixture was extracted with ethyl acetate twice. The combined organic layer was washed with brine, dried over magnesium sulfate and evaporated under reduced pressure. The residue was purified by column chromatography (silica gel 25 g, n-hexane:dichloromethane=1:1) to give 2-chloro-1-(4-methylpyridin-2-yl)propan-1-one (0.71 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06521643B1 |
| 出典データセット | uspto-grants-2003_02 |
| ORD ID | ord-85ffa0499c814ce1bfe6c4a830ea5708 |
| 出典メモ | uspto-grants-2003_02 |