関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 4-Toluenesulfonyl chloride | HCID 7397 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 2-Fluoroethanol | HCID 9737 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 2-Fluoroethyl p-Toluenesulfonate | HCID 256019 | 78% |
反応手順
To a stirred solution of 2-fluoroethanol (1.92 g, 29.97 mmol) in dry pyridine (15 ml) under an atmosphere of argon at 0° C. was added p-toluenesulphonyl chloride over 15 min, maintaining the temperature below 5° C. The reaction mixture was then stirred at 0° C. for 4 h, then at room temperature for 12 h. The reaction mixture was cooled to 0° C. and ice (15 g) was added followed by water (40 ml) and EtOAc (50 ml). The organic extract was washed with water (30 ml), 1 M HCl (until aqueous extracts were acidic), 10% sodium carbonate (2×30 ml), brine (40 ml) and dried (Na2SO4). The solvent was removed under reduced pressure to give the title compound (5.10 g, 78%) as a colourless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08895313B2 |
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| 出典データセット | uspto-grants-2014_11 |
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| ORD ID | ord-3b1adff8ea8a40a198aa5711e8a6cac8 |
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| 出典メモ | uspto-grants-2014_11 |
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