化工社化工社 化学情報印刷レポート · 研究参考用
Water → 4-acetyl-N-(tert-butyldimethylsiloxy)benzenesulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-Acetylbenzenesulfonyl chloride | HCID 266418 | — |
| 反応物 | O-(tert-Butyldimethylsilyl)hydroxylamine | HCID 4691350 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-acetyl-N-(tert-butyldimethylsiloxy)benzenesulfonamide | HCID 21082528 | 78.9% |
反応手順
Ex-33A: To a solution of O-(tert-butyldimethylsilyl)hydroxylamine (0.74 g, 5 mmol) and triethylamine (1.01 g, 10 mmol) in 25 ml THF, 4-acetylbenzenesulfonyl chloride(1.1 g, 5 mmol) was added at 0° C. The mixture was stirred overnight and then poured into H2O. The precipitate was filtered, dried, and recrystallized from EtOAc/Hexene to give 1.3 g (76.8%) of 4-acetyl-N-(tert-butyldimethylsiloxy)benzenesulfonamide as a white solid. 1H-NMR (300 MHz, CDCl3) δ 8.11 (d, J=9 Hz, 2H), 8.01 (d, J=9 Hz, 2H), 6.59 (b, 1H), 2.67 (s, 3H), 0.89 (s, 9H), 0.20 (s, 6H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07173129B2 |
| 出典データセット | uspto-grants-2007_02 |
| ORD ID | ord-8405d919c0c34009802b017a6c56ebd7 |
| 出典メモ | uspto-grants-2007_02 |