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Triethylamine → 10-[4-[(Diphenylphosphinyl)amino]benzoyl]-10,11-dihydro-5H-pyrrolo-[2,1-c][1,4]benzodiazepine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Diphenylphosphinic chloride | HCID 73910 | — |
| 反応物 | 10,11-dihydro-10(4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine | HCID 10828280 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 10-[4-[(Diphenylphosphinyl)amino]benzoyl]-10,11-dihydro-5H-pyrrolo-[2,1-c][1,4]benzodiazepine | HCID 15340678 | 96.4% |
反応手順
A mixture of 0.10 g of 10,11-dihydro-10-(4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine 0.060 g of triethylamine and 0.12 g of diphenylphosphinyl chloride in 2 ml of dichloromethane is stirred at room temperature for 2 hours and then 1N NaOH is added. The mixture is extracted with ethyl acetate and the extract washed with brine and dried (Na2SO4). The solvent is removed and the residue triturated with ether-hexane to give 0.16 g of a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05624923 |
| 出典データセット | uspto-grants-1997_04 |
| ORD ID | ord-7f879c8a8195417d942705d62cb9948d |
| 出典メモ | uspto-grants-1997_04 |