化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → 1-(2-Chloro-4-nitrobenzyl)-4-methylpiperazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1-Methylpiperazine | HCID 53167 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 1-(Bromomethyl)-2-chloro-4-nitrobenzene | HCID 3016368 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(2-Chloro-4-nitrobenzyl)-4-methylpiperazine | HCID 66735814 | 86.6% |
反応手順
To a solution of crude 1-(bromomethyl)-2-chloro-4-nitro-benzene (29.1 mmol; 50% pure) in 30 mL of DCM was added Et3N (4.2 mL, 30 mmol) and 1-methylpiperazine (3.4 mL, 30 mmol). After stirring for 3 h at ambient temperature, aq. NaHCO3 was added and the mixture was extracted with DCM. The combined organic layer was dried over Na2SO4, filtered, concentrated, and the resulting residue was purified by silica gel chromatography (eluted with 5% MeOH/DCM) to provide 6.80 g of product as a dark yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09029533B2 |
| 出典データセット | uspto-grants-2015_05 |
| ORD ID | ord-6437dee56f534ba69acbb49c8b5920b1 |
| 出典メモ | uspto-grants-2015_05 |