化工社化工社 化学情報印刷レポート · 研究参考用
Ethylene Glycol → 2-((7-Bromoquinoxalin-2-yl)oxy)ethanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethylene Glycol | HCID 174 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 7-Bromo-2-chloroquinoxaline | HCID 4913253 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-((7-Bromoquinoxalin-2-yl)oxy)ethanol | HCID 59710030 | 85% |
反応手順
Suspend sodium hydride (310 mg, 13 mmol) in a solution of ethylene glycol (800 mg, 13 mmol) in DMF (50 mL) at 0° C. After stirring for 30 min at room temperature, 7-bromo-2-chloro-quinoxaline (Preparation 26; 610 mg, 2.5 mmol) is added. Stir for 2 h at room temperature and dilute with 3:1 chloroform/isopropyl alchol. Wash the organic phase with brine and purify by FCC to give the title compound (564 mg, 85%). MS m/e (268, M+1). 1H NMR (400 MHz, CDCl3) δ 8.5 (s, 1H), 8.0 (d, J=2.0 Hz), 7.90 (dd, J=8.8, 2.0 Hz, 1H), 7.7 (d, J=8.8 Hz, 1H), 4.6 (t, d=4.8 Hz, 2H), 43.9 (t, J=4.8 Hz, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07405299B2 |
| 出典データセット | uspto-grants-2008_07 |
| ORD ID | ord-a6e08bfc6bc34bd0849c9c54ebc3f561 |
| 出典メモ | uspto-grants-2008_07 |