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Triethylamine → N-[5-(5H-Pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)ylcarbonyl)-2-pyridinyl]-2-methylbenzeneacetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | o-Tolyl-acetyl chloride | HCID 2760632 | — |
| 反応物 | 10, 11-dihydro-10-(6-amino-3-pyridinylcarbonyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine | HCID 18917501 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-[5-(5H-Pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)ylcarbonyl)-2-pyridinyl]-2-methylbenzeneacetamide | HCID 18917528 | — |
反応手順
A mixture of 2.0 mmol of 10,11-dihydro-10-(6-amino-3-pyridinylcarbonyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine, 2.1 mmol of 2-methylbenzeneacetyl chloride and 5 mmol of triethylamine in 10 ml of dichloromethane is stirred under argon at room temperature for 16 hours. The solvent is removed under vacuum and the residue partitioned between 50 ml of ethyl acetate and 25 ml of water. The organic layer is separated, washed with H2O, 1N NaHCO3, brine and dried (Na2SO4). The solvent is removed and the residue chromatographed on silica gel with ethyl acetate-hexane as solvent to give the product as a solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05612334 |
| 出典データセット | uspto-grants-1997_03 |
| ORD ID | ord-08f31ee8f77a4599b0ad743ed3bda9b7 |
| 出典メモ | uspto-grants-1997_03 |