関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Dithionite | HCID 24489 | — |
| 反応物 | 1,3-dimethyl-1H-pyrazole-4-carbaldehyde | HCID 847285 | — |
| 反応物 | 5-Chloro-4-(4-(4-chlorobenzyl)piperazin-1-yl)-3-nitropyridin-2-amine | HCID 57897254 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | HCID 178434000 | HCID 178434000 | — |
反応手順
To a mixture of 5-chloro-4-(4-(4-chlorobenzyl)piperazin-1-yl)-3-nitropyridin-2-amine (0.076 g, 0.20 mmol) and EtOH (4.0 mL) was added 1,3-dimethyl-1H-pyrazole-4-carbaldehyde (0.027 g, 0.22 mmol) followed by a freshly prepared aqueous solution of Na2S2O4 (1M; 0.85 mL, 0.85 mmol). The reaction mixture was stirred at 80° C. for 24 h, it was then allowed to cool to room temperature, concentrated in vacuo, and the residue was absorbed on silica gel and placed on a 10 g isolute silica column. Elution with ethyl acetate/dichloromethane (v/v; 1:1), and then 4% methanol in ethyl acetate/dichloromethane (v/v; 1:1) afforded the title compound as a white solid after trituration with diethyl ether (0.023 g, 25%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09447092B2 |
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| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-e9fbdd2da7994bfc8862a96b29e04a89 |
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| 出典メモ | uspto-grants-2016_09 |
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