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N-bromobutanimide → HCID 178509106、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | 3-(3-chlorophenyl)-1H-pyrazol-5-amine | HCID 178507281 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 178509106 | HCID 178509106 | 80.4% |
反応手順
To a stirring solution of 5-(3-chloro-phenyl)-2H-pyrazol-3-ylamine (1.53 g, 7.9 mmol) in THF (32 mL) was added N-bromosuccinimide (1.55 g, 8.7 mmol). The reaction mixture was stirred for 5 h at room temperature, then absorbed on silica gel. Purification on silica gel with 0-10% MeOH in CH2Cl2 as eluent provided 1.73 g (80%) of 4-bromo-5-(3-chloro-phenyl)-2H-pyrazol-3-ylamine as a brown solid. 1H NMR (d6-DMSO) δ: 12.2 and 12.4 (2 broad s, 1H, NH+tautomer), 7.77 (s, 1H), 7.73 (broad s, 1H), 7.48 (broad s, 1H), 7.43 (broad s, 1H), 5.30 (broad s, 1H, NH), 4.82 (broad s, 1H, NH); HPLC/MS m/z: 272 [MH]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07473783B2 |
| 出典データセット | uspto-grants-2009_01 |
| ORD ID | ord-ef0b2e83705d4219bba27c2ad6fce27e |
| 出典メモ | uspto-grants-2009_01 |