化工社化工社 化学情報印刷レポート · 研究参考用
Potassium Carbonate → 1-(2-Hydroxyethyl)-4-(2-fluorophenyl)piperazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Iodoethanol | HCID 12225 | — |
| 反応物 | 1-(2-Fluorophenyl)piperazine | HCID 70529 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-(2-Hydroxyethyl)-4-(2-fluorophenyl)piperazine | HCID 20635175 | 65.9% |
反応手順
A mixture of 1-(2-fluorophenyl)piperazine (0.50 g), 2-iodoethanol (0.48 g), and potassium carbonate (1.5 g) in dimethylformamide (7 mL) was heated at reflux for three hours. The solvent was removed in vacuo and the residue was purified by preparative thin-layer chomatography (silica gel, eluting with chloroform/methanol, 9:1), giving the title compound as a yellow oil (0.41 g, 65%). 1H NMR (300 MHz, CDCl3) δ7.09-6.90 (m, 4H), 3.67 (t, 2H, J=5.4 Hz), 3.13 (t, 4H, J=4.7 Hz), 2.76 (br s, 1H), 2.71 (t, 4H, J=4.8 Hz), 2.63 (t, 4H, J=5.4 Hz). 13C NMR (75 MHz, CDCl3) δ156.3 (d, J=244.1 Hz), 140.6 (d, J=8.8 Hz), 125.1 (d, J=3.4 Hz), 123.2 (d, J=8.1 Hz), 119.5 (d, J=2.9 Hz), 116.7 (d, J=20.6 Hz), 60.1, 58.4, 53.6 (2C), 51.2 (d, 2C, J=3.0 Hz).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06706716B2 |
| 出典データセット | uspto-grants-2004_03 |
| ORD ID | ord-74e89468e2c345a2a19678b9a39c2698 |
| 出典メモ | uspto-grants-2004_03 |