関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-Methylpiperazine | HCID 53167 | — |
| 反応物 | 5-Fluoro-2-nitrotoluene | HCID 94956 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 1-Methyl-4-(3-methyl-4-nitrophenyl)piperazine | HCID 18439747 | — |
反応手順
A mixture of 5-fluoro-2-nitrotoluene (2.5 g, 16 mmol), N-methylpiperazine (2 mL, 18 mmol) and potassium carbonate (2.7 g, 19 mmol) in DMSO (7 mL) was stirred and heated at 100° C. for 2 hours. The reaction mixture was cooled to ambient temperature and then diluted with ethyl acetate (100 mL), washed with water (3×30 mL), brine, dried (MgSO4) and concentrated in vacuo. The resultant crude product was purified by flash chromatography on SiO2 eluting with dichloromethane—40% methanol/dichloromethane (gradient) to afford the desired title compound as a yellow solid, 3.67 g, 97%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08916591B2 |
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| 出典データセット | uspto-grants-2014_12 |
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| ORD ID | ord-1d672d88ecbf4736a2de59c410b2895e |
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| 出典メモ | uspto-grants-2014_12 |
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