関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sulfuryl chloride | HCID 24648 | — |
| 反応物 | 2,3-Dimethylanisole | HCID 76269 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-Methoxy-2,3-dimethylbenzenesulfonyl chloride | HCID 20689151 | 94.3% |
反応手順
2,3-Dimethylanisole (1 cm3, 7.23 mmol) was dissolved into dichloromethane (4 cm3) and cooled to 0° C. Chlorosulfonyl chloride (2 cm3, 30.0 mmol) was then added dropwise, over 10 min and once the addition was completed the mixture was allowed to warm to room temperature and stirred for a further 45 min. The reaction was then quenched by the slow addition of ice/water (50 cm3, CARE, exotherm) before further dichloromethane (30 cm3) and water (30 cm3) were added and the organic layer was collected. The aqueous layer was washed with dichloromethane (15 cm3) and then organic extracts were combined and washed with saturated aqueous sodium chloride solution (70 cm3) before being dried over sodium sulfate. The solvent was evaporated under reduced pressure to afford title compound (1.6 g, 6.82 mmol, 94% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07838518B2 |
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| 出典データセット | uspto-grants-2010_11 |
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| ORD ID | ord-1a5e44fa474642838b6f1af30a12104c |
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| 出典メモ | uspto-grants-2010_11 |
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