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Thionyl Chloride → 4-Phenoxybenzene-1-sulfonyl chloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 4-phenoxybenzenesulfonic Acid | HCID 11081501 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-Phenoxybenzene-1-sulfonyl chloride | HCID 2794756 | — |
反応手順
The sulphonic acid (2a) was dissolved in an excess of thionyl chloride (30 mL), a catalytic amount of DMF (cat) was added, and the resulting mixture was stirred for 6 h at reflux. The solvent was evaporated and the residue dissolved in Et20 (40 mL). The ether solution was washed with 5% aqueous NaOH (3×40 mL) and water (6×40 mL), dried over anhydrous MgSO4, filtered, and concentrated in vacuo. After drying in high vacuum overnight, the pure product was obtained as a white solid. Yield 63%: 2.09 g, 7.44 mmol, (light yellow syrup). 1H-NMR (CDCl3): δ 7.44 (d, 3J=9.1 Hz, 2H, ArH), 7.38 (d, 3J=9.1 Hz, 2H, ArH), 7.19 (t, 1H, ArH), 7.12 (d, 3J=9.1 Hz, 2H, ArH), 6.98 (d, 3J=9.1 Hz, 2H, ArH)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08524194B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-54b763fa48f0470b873aab1b94d435ed |
| 出典メモ | uspto-grants-2013_09 |