Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Chloroacetyl chloride → 2-chloro-N-[4-(5H-pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)ylcarbonyl)phenyl]acetamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Chloroacetyl chloride | HCID 6577 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 10,11-dihydro-10(4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine | HCID 10828280 | — |
| 촉매 | 2-Dimethylaminopyridine | HCID 21885 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 2-chloro-N-[4-(5H-pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)ylcarbonyl)phenyl]acetamide | HCID 21837075 | 100.1% |
반응 단계
To a stirred solution of 0.91 g of 10,11-dihydro-10-(4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine in 10 ml of methylene chloride is added 0.46 g of triethylamine and 36 mg of dimethylaminopyridine followed by the slow addition of 0.42 g of chloroacetyl chloride in 5 ml of methylene chloride. The resulting mixture is stirred at room temperature for 3 hours then partitioned with 10 ml of 50% NaHCO3 and the methylene chloride evaporated in vacuo. The remaining suspension is filtered, washed with 50% NaHCO3, H2O, EtOAc (2×2 ml), ether (2×5 ml) and dried in vacuo to give 1.14 g of beige solid. MS(CI): 380(M+H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05624923 |
| 출처 데이터셋 | uspto-grants-1997_04 |
| ORD ID | ord-27ec54cf48b14a64ba0782b9e419ea70 |
| 출처 메모 | uspto-grants-1997_04 |