関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Chlorosulfonic acid | HCID 24638 | — |
| 反応物 | ((S)-2-Fluoro-1-methyl-ethyl)-benzene | HCID 53628601 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-((S)-2-Fluoro-1-methyl-ethyl)-benzenesulfonyl chloride | HCID 53628600 | 25% |
反応手順
3.5 g of ((S)-2-fluoro-1-methyl-ethyl)-benzene (25.32 mmol) were dissolved in 80 ml of dichloromethane. At 0-5° C., 11.81 g of chlorosulfonic acid (101.31 mmol), dissolved in 20 ml of dichloromethane, were added dropwise. The reaction mixture was stirred for 30 min at room temperature and 2 h at 30° C. The solvent was evaporated. 150 ml of diethyl ether were added to the residue, washed once with 150 ml of water, and the organic layer was dried over magnesium sulfate, filtered, and the solvent evaporated under reduced pressure. The crude product was purified via silica gel chromatography with n-heptane-dichloromethane (6:4) as eluent to give 1.5 g of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08486984B2 |
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| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-4254be179a7943c58c49a5be92dff354 |
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| 出典メモ | uspto-grants-2013_07 |
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