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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 1 N 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 | US05968930 |
| 出典データセット | uspto-grants-1999_10 |
| ORD ID | ord-1313b32c5b8543f19a71f3cbbe654690 |
| 出典メモ | uspto-grants-1999_10 |