関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-Methylpiperazine | HCID 53167 | — |
| 反応物 | 2-Chloro-5-nitropyridine | HCID 78308 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-Methyl-4-(5-nitropyridin-2-yl)piperazine | HCID 2764066 | 90% |
反応手順
A stirred mixture of 2-chloro-5-nitropyridine (3.16 g, 20.0 mmol), 1-methyl-piperazine (2.00 g, 2.00 mmol) and potassium carbonate (2.76 g, 20.0 mmol) in DMF is heated at 100° C. for 24 h, cooled, poured into water and extracted with CH2Cl2. The combined extracts are dried over MgSO4 and concentrated in vacuo. The resultant residue is purified by flash chromatography (SiO2, 2% ammonia in 10:90 ethanol:ethyl acetate as eluent) affords the title compound as an off-white solid, 4.0 g (90% yield), identified by NMR analysis.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07259165B2 |
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| 出典データセット | uspto-grants-2007_08 |
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| ORD ID | ord-ffc0e54e765c4103a76baaa42ef2a001 |
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| 出典メモ | uspto-grants-2007_08 |
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