化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → 4-(Biphenyl-2-yloxy)-3-cyanobenzenesulfonyl chloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Hypochlorite | HCID 23665760 | — |
| 反応物 | 5-Benzylsulfamyl-2-(biphenyl-2-yloxy)-benzonitrile | HCID 66905456 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-(Biphenyl-2-yloxy)-3-cyanobenzenesulfonyl chloride | HCID 59436506 | — |
反応手順
A mixture of 5-benzylsulfamyl-2-(biphenyl-2-yloxy)-benzonitrile (Preparation 56, 6.06 g, 15.4 mmol), dichloromethane and aq HCl was stirred vigorously with cooling (ice bath). Sodium hypochlorite was added dropwise over 30 minutes and stirring continued with cooling for 1 hour. The layers were separated, the aqueous extracted with dichloromethane (2×100 ml), and the organic collected, dried (MgSO4) and concentrated in vacuo. The residue was purified using silica gel column chromatography (ethyl acetate:Heptane 10/90 to 20/80) to furnish 4.58 g of the title compound. 1HNMR (CDCl3): δ 6.7 (m, 1H), 7.2-7.6 (m, 9H), 7.85 (m, 1H), 8.15 (m, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08541588B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-3ec879e18afb4ac9b07b7d7538aaf8b3 |
| 出典メモ | uspto-grants-2013_09 |