化工社化工社 化学情報印刷レポート · 研究参考用
Dibenzylamine → (E)-N,N,N',N'-tetrabenzylbut-2-enediamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dibenzylamine | HCID 7656 | — |
| 反応物 | Fumaryl chloride | HCID 5325504 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (E)-N,N,N',N'-tetrabenzylbut-2-enediamide | HCID 86722949 | 94.3% |
反応手順
To a cooled (−5° C.) solution of N,N-dibenzylamine (19.3 mL, 100 mmol) in DCM (200 mL) is added TEA (13.8 mL, 100 mmol). To this solution is added, drop wise over 5 minutes, fumaroyl chloride (4.2 mL, 40 mmol). On complete addition, the cold bath is removed and stirring continued for 1 hr. This solution is diluted with DCM, washed with HCl (approx. 100 mL of 1M aq.) then water (2×), dried over MgSO4 and concentrated. The solid residue is crystallized from hot (109° C.) toluene to give the title compound (17.9 g) as a white solid. ESI-MS (m/z) 475 (MH)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08912169B2 |
| 出典データセット | uspto-grants-2014_12 |
| ORD ID | ord-873f164e835244a9ae247159ab8e4c78 |
| 出典メモ | uspto-grants-2014_12 |