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4-Methylbenzenethiol → 1-Acetoxy-3-(4-methylphenylthio)acetone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Methylbenzenethiol | HCID 7811 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Propanone, 1-(acetyloxy)-3-chloro- | HCID 38413 | — |
| 溶媒 | tert-Butyl methyl ether | HCID 15413 | — |
| 生成物 | 1-Acetoxy-3-(4-methylphenylthio)acetone | HCID 68284616 | 97.6% |
反応手順
To a solution of 1-acetoxy-3-chloroacetone (5.0 g, 33.2 mmol) and 4-methylthiophenol (4.12 g, 33.2 mmol) in tert-butyl methyl ether (100 ml) was slowly added triethylamine (5.1 ml, 36.6 mmol) under ice-cooling. The solution was stirred at room temperature for 30 minutes. The reaction solution was washed with water, saturated aqueous sodium hydrogen carbonate solution, then saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=7:3) to give 7.72 g of 1-acetoxy-3-(4-methylphenylthio)acetone (yield: 97%) as oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09029295B2 |
| 出典データセット | uspto-grants-2015_05 |
| ORD ID | ord-0358b8ce5dcc4b9b830d8276f3ec09a8 |
| 出典メモ | uspto-grants-2015_05 |