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三乙胺 → N-[4-(3-Chloro-5H-pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)ylcarbonyl)phenyl]-2-methylbenzamide
参与物
| 角色 | 名称 | HCID | 投料 |
|---|---|---|---|
| 反应物 | 三乙胺 | HCID 8471 | — |
| 反应物 | methylbenzoyl chloride | HCID 70276 | — |
| 反应物 | 3-Chloro-10,11-dihydro-10-(4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine | HCID 21837099 | — |
| 溶剂 | 二氯甲烷 | HCID 6344 | — |
| 产物 | N-[4-(3-Chloro-5H-pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)ylcarbonyl)phenyl]-2-methylbenzamide | HCID 21836983 | — |
反应步骤
A mixture of 1 mmol of 3-chloro-10,11-di-hydro-10-(4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine, 2 mmol of triethylamine, and 1.1 mmol of 2-methylbenzoylchloride in 8 ml of dichloromethane is stirred at room temperature overnight. The mixture is washed with water, and 1M NaHCO3 and dried(Na2SO4). The solvent is removed in vacuo to give a solid which is recrystallized from dichloromethane-hexane to give crystals, 185°-187° C.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 专利号 | US05624923 |
| 来源数据集 | uspto-grants-1997_04 |
| ORD ID | ord-03a6b4230016431fa7c2b186b3613d08 |
| 来源说明 | uspto-grants-1997_04 |