Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dibenzylamine → (E)-N,N,N',N'-tetrabenzylbut-2-enediamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dibenzylamine | HCID 7656 | — |
| 반응물 | Fumaryl chloride | HCID 5325504 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | (E)-N,N,N',N'-tetrabenzylbut-2-enediamide | HCID 86722949 | 94.3% |
반응 단계
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)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08912169B2 |
| 출처 데이터셋 | uspto-grants-2014_12 |
| ORD ID | ord-873f164e835244a9ae247159ab8e4c78 |
| 출처 메모 | uspto-grants-2014_12 |