関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Stannous chloride dihydrate | HCID 61436 | — |
| 反応物 | 6,7-dihydro-5-(2-chloro-4-nitrobenzoyl)-5H-pyrrolo[1,2-a][1,5]benzodiazepine | HCID 21837030 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 6,7-Dihydro-5-(4-amino-2-chlorobenzoyl)-5H-pyrrolo[1,2-a][1,5]benzodiazepin | HCID 21836994 | 102.3% |
反応手順
To a solution of 0,50 g of 6,7-dihydro-5-(2-chloro-4-nitrobenzoyl)-5H-pyrrolo[1,2-a][1,5]benzodiazepine in 10 ml of ethyl alcohol and 2 ml of tetrahydrofuran is added 2.35 g of SnCl2.2H2O and the mixture stirred at 55° C. for 30 minutes. The solvents are evaporated in vacuo to a residue which is stirred with 20 ml of 1N NaOH and 40 ml of ethyl acetate for 15 minutes and filtered through diatomaceous earth. The filter pad is washed with 2×10 ml of ethyl acetate and the combined extracts washed with brine, dried (Na2SO4) and evaporated in vacuo to give 0.47 g of solid residue which is triturated with ether-hexane to give 0.43 g of light yellow crystalline solid. MS(CI): 338 (M+H, Cl35) 340 (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-5d66cdab1c794ab784689ff5a3d4e879 |
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| 出典メモ | uspto-grants-1998_03 |
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