化工社化工社 化学情報印刷レポート · 研究参考用
4-Nitrobenzyl chloride → 1-Isopropyl-4-(4-nitrobenzyl)piperazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Nitrobenzyl chloride | HCID 7482 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-Isopropylpiperazine | HCID 78013 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 1-Isopropyl-4-(4-nitrobenzyl)piperazine | HCID 882651 | 90.6% |
反応手順
A mixture of 4-nitrobenzylchloride (4.1 g, 23.90 mmol), N-isopropylpiperazine (3.6 g, 28.67 mmol, 1.2 equiv), potassium carbonate (6.5 g, 47.79 mmol, 2 equiv) and acetone (82 ml) was stirred for 16 h at reflux. The reaction mixture was allowed to cool, was then filtered and concentrated. The residue was purified by silica gel column chromatography (DCM/MeOH+1% NH3aq, 9:1) to afford 5.7 g of the title compound: ESI-MS: 264.1 [M+H]+; TLC: tR=1.73 min (System 1); TLC: Rf=0.34 (DCM/MeOH+1% NH3aq, 9:1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08536175B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-078e0ec21f6f4cd6a82c0fa59bcb545b |
| 出典メモ | uspto-grants-2013_09 |