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Water → 6,7-dihydro-5H-pyrrolo[1,2-a][1,5]benzodiazepine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 6,7-dihydro-5H-pyrrolo[1,2-a][1,5]benzodiazepin-6-one | HCID 12359340 | — |
| 反応物 | Diborane dimethylsulfide | HCID 22038413 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 6,7-dihydro-5H-pyrrolo[1,2-a][1,5]benzodiazepine | HCID 12359341 | 99.9% |
反応手順
To a solution of 0.070 g of 6,7-dihydro-5H-pyrrolo[1,2-a][1,5]benzodiazepin-6-one in 2 ml of tetrahydrofuran is added 0.45 ml of a 2.0M solution of diborane-dimethylsulfide in tetrahydrofuran. The mixture is refluxed for 3 hours, poured into water and made basic with 2N NaOH. The tetrahydrofuran is removed under vacuum and the residual aqueous mixture extracted with diethyl ether. The extract is washed with brine, dried (Na2SO4) and the solvent removed to give 0.065 g of a colorless oil; one spot by thin layer chromatography (silica gel) with ethyl acetate-hexane (1:2) as solvent (Rf 0.81).
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-8b2a26cfe0734d588ff79f3675b6a12e |
| 出典メモ | uspto-grants-1997_03 |