化工社化工社 化学情報印刷レポート · 研究参考用
Sodium Hydroxide → 3-Bromoimidazo(1,2-b)pyridazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | Imidazo(1,2-b)pyridazine | HCID 136599 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 3-Bromoimidazo(1,2-b)pyridazine | HCID 12872319 | — |
反応手順
Bromine (0.649 mL, 12.6 mmol) was added dropwise to a stirred mixture of Imidazo[1,2-b]pyridazine (1.0 g, 8.39 mmol) in acetic acid (42 ml) and the mixture was stirred at room temperature for 1 h. The mixture was neutralized with 1 N sodium hydroxide (100 mL) and solid sodium hydroxide, poured into ethyl acetate and sodium bicarbonate solution, and extracted with ethyl acetate (3×200 mL). The combined organics were washed with brine, dried (MgSO4), and concentrated to afford the title compound. 1H NMR (600 MHz, CD3SOCD3) δ 8.66 (d, 1H); 8.17 (d, 1H); 7.93 (s, 1H); 7.31 (dd, 1H). LRMS (APCI) calc'd for (C6H5BrN3) [M+H]+, 198.0. found 198.0.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08592425B2 |
| 出典データセット | uspto-grants-2013_11 |
| ORD ID | ord-891d5284fa094b1f980f86328bdd5ba6 |
| 出典メモ | uspto-grants-2013_11 |