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Magnesium orthosilicate → Biphenyl-2-carboxylic acid [4-(5H,11H-benzo[e]pyrrolo[1,2-a][1,4]diazepine-10-carbonyl)-3-chloro-phenyl]-amide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Magnesium orthosilicate | HCID 66225 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 10,11-Dihydro-5H-benzo[e]pyrrolo[1,2-a][1,4]diazepine | HCID 15547048 | — |
| 反応物 | 4-[([1,1'-Biphenyl]-2-carbonyl)amino]-2-chlorobenzoyl chloride | HCID 22099600 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 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% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05753648 |
| 出典データセット | uspto-grants-1998_05 |
| ORD ID | ord-7e30c25978cb4f1596ee6bc23b3b2490 |
| 出典メモ | uspto-grants-1998_05 |