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Ethanolamine → HCID 66672990、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanolamine | HCID 700 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-Bromo-2,5-difluorobenzenesulfonyl Chloride | HCID 574590 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 66672990 | HCID 66672990 | 70% |
反応手順
A solution of 4-bromo-2,5-difluorobenzenesulfonyl chloride (1.17 g, 4 mmol) in CH2Cl2 (3 mL) was added to a solution of 2-aminoethanol (0.36 mL, 6 mmol) and triethylamine (1.67 mL, 12 mmol) in CH2Cl2 (12 mL) at ambient temperature. The mixture was stirred at ambient temperature for 1 h and concentrated. The crude product was purified by chromatography on a silica gel column using 0 to 10% MeOH/CH2Cl2 to give 884 mg (70%) of 4-bromo-2,5-difluoro-N-(2-hydroxyethyl)benzenesulfonamide as a white solid. 1H NMR (400 MHz, CDCl3): δ 7.67 (dd, 1H, Ja=7.2 Hz, Jb=6.0 Hz), 7.47 (dd, 1H, Ja=8.7 Hz, Jb=5.1 Hz), 5.39-5.14 (m, 1H), 3.78-3.64 (m, 2H), 3.26-3.10 (m, 2H), 1.73 (bs, 1H); LRMS (ESI), m/z 314/316 (M−H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08101634B2 |
| 出典データセット | uspto-grants-2012_01 |
| ORD ID | ord-87786cc817af465faaa129b5807fca39 |
| 出典メモ | uspto-grants-2012_01 |