関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 1-(2-Methylpropyl)piperazine | HCID 2052052 | — |
| 反応物 | 5-Bromo-4-chloro-3-nitropyridin-2-amine | HCID 45480236 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | 5-Bromo-4-(4-isobutylpiperazin-1-yl)-3-nitropyridin-2-amine | HCID 46868348 | — |
反応手順
To a mixture of 5-bromo-4-chloro-3-nitro-pyridin-2-ylamine (0.126 g, 0.50 mmol) and isopropanol (9 ml) was added 1-isobutylpiperazine (0.078 g, 0.55 mmol) with the aid of isopropanol (5 ml) followed by diisopropylethylamine (0.10 ml, 0.57 mmol). The reaction mixture was heated at 45° C. for 20 h, then allowed to cool to room temperature. The precipitate was collected by filtration and washed with isopropanol and diethyl ether. The title compound was thus obtained as a yellow solid (0.112 g, 63%). 1H-NMR (500 MHz, DMSO-d6) 0.87 (d, J=6.56 Hz, 6H, CH(CH3)2), 1.77 (m, 1H, CH(CH3)2), 2.08 (d, J=7.35 Hz, 2H, N—CH2), 2.47 (br s, 4H, piperazine N(CH2)2), 3.04 (br s, 4H, piperazine N(CH2)2), 6.96 (s, 2H, NH2), 8.15 (s, 1H, 6-H);
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08088761B2 |
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| 出典データセット | uspto-grants-2012_01 |
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| ORD ID | ord-b733c04c79214e358a1452188a150f9d |
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| 出典メモ | uspto-grants-2012_01 |
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