関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Benzoyl chloride, 2-chloro-4-nitro- | HCID 81522 | — |
| 反応物 | 6,7-dihydro-5H-pyrrolo[1,2-a][1,5]benzodiazepine | HCID 12359341 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 6,7-dihydro-5-(2-chloro-4-nitrobenzoyl)-5H-pyrrolo[1,2-a][1,5]benzodiazepine | HCID 21837030 | 105.6% |
反応手順
To a solution of 0.28 g of 6,7-dihydro-5H-pyrrolo[1,2-a][1,5]benzodiazepine in 6 ml of methylene chloride is added 0.30 g of triethylamine followed by 0.50 g of 2-chloro-4-nitrobenzoyl chloride in 0.5 ml of methylene chloride. The reaction mixture is stirred at room temperature for 1 hour then quenched with 5 ml of saturated NaHCO3. The methylene chloride is evaporated in vacuo and the residue is diluted with 5 ml of water and extracted with 20 ml of ethyl acetate. The organic layer is separated washed with saturated NaHCO3 and brine, dried with Na2SO4 and evaporated in vacuo to give 0.59 g of a yellow foam which is triturated with ether-hexanes to give 0.56 g of the desired product as off-white solid. MS(CI): 368(M+H)(Cl35) 370 (M+H) (Cl37)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05733905 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-fa4012fada9d450bb1c4694877c81d19 |
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| 出典メモ | uspto-grants-1998_03 |
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