Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → N-(2,3-Dimethylphenyl)-4-(5H-pyrrolo[2,1-c][1,4]-benzodiazepin-10(11H)-ylcarbonyl)benzamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 4-(5H-pyrrolo[2,1-c]-[1,4]benzodiazepin-10(11H)-ylcarbonyl)benzoic acid | HCID 9905628 | — |
| 반응물 | Diethylphosphorylcyanide | HCID 13586794 | — |
| 반응물 | Benzenamine, ar,ar-dimethyl-, hydrochloride (1:1) | HCID 22239262 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | N-(2,3-Dimethylphenyl)-4-(5H-pyrrolo[2,1-c][1,4]-benzodiazepin-10(11H)-ylcarbonyl)benzamide | HCID 21837120 | 25.4% |
반응 단계
A mixture of 0.332 g of 4-(5H-pyrrolo[2,1-c]-[1,4]benzodiazepin-10(11H)-ylcarbonyl)benzoic acid, 0.222 g of triethylamine, 0.157 g of 2,3-dimethylaniline hydrochloride, 0.15 ml of diethylphosphoryl cyanide in 20 ml of dichloromethane is heated on a steam bath for 3 hours. The mixture is washed with H2O, 1M NaHCO3, H2O, 1N HCl, brine and dried (Na2SO4). The solution is filtered through a thin pad of hydrous magnesium silicate and the filter cake washed with dichloromethane. The filtrate is concentrated to dryness under vacuum and the residue crystallized from dichloromethane-hexane to give 0.11 g of crystals, m.p. 239°-240° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05854237 |
| 출처 데이터셋 | uspto-grants-1998_12 |
| ORD ID | ord-c162532d97c94fa1b08f84c650e7a90c |
| 출처 메모 | uspto-grants-1998_12 |