Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Magnesium orthosilicate → Biphenyl-2-carboxylic acid [4-(5H,11H-benzo[e]pyrrolo[1,2-a][1,4]diazepine-10-carbonyl)-3-chloro-phenyl]-amide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Magnesium orthosilicate | HCID 66225 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 10,11-Dihydro-5H-benzo[e]pyrrolo[1,2-a][1,4]diazepine | HCID 15547048 | — |
| 반응물 | 4-[([1,1'-Biphenyl]-2-carbonyl)amino]-2-chlorobenzoyl chloride | HCID 22099600 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | Biphenyl-2-carboxylic acid [4-(5H,11H-benzo[e]pyrrolo[1,2-a][1,4]diazepine-10-carbonyl)-3-chloro-phenyl]-amide | HCID 10459252 | 75.2% |
반응 단계
To a solution of 0.52 g of 10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine and 0.39 g of N,N-diisopropylethylamine in 25 ml of methylene chloride is added 1.1 g of 4-[([1,1'-biphenyl]-2-carbonyl)amino]-2-chlorobenzoyl chloride followed by stirring at room temperature for 18 hours. The reaction mixture is washed with water and saturated aqueous NaHCO3 and the organic layer dried(Na2SO4). The organic layer is passed through hydrous magnesium silicate and the filtrate concentrated in vacuo to give a residue which is dissolved in methylene chloride and passed through hydrous magnesium silicate two additional times to give upon concentration in vacuo 1.10 g of the desired product as a residue. M+ =516,518,520.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05753648 |
| 출처 데이터셋 | uspto-grants-1998_05 |
| ORD ID | ord-7e30c25978cb4f1596ee6bc23b3b2490 |
| 출처 메모 | uspto-grants-1998_05 |