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 | 5-Chloro-2-nitroaniline | HCID 74218 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 5-(4-Methylpiperazin-1-yl)-2-nitroaniline | HCID 2760034 | 54.4% |
反応手順
A mixture of 5-chloro-2-nitrophenylamine (2.5 g, 14 mmol), 1-methylpiperizine (3.2 mL, 30 mmol), and potassium carbonate (K2CO3) (2.0 g, 14 mmol) in dimethylformamide (DMF) (20 mL) was stirred at 120° C. for 18 h. The reaction mixture was cooled to room temperature and poured into water (150 mL). The precipitated crude product was collected by filtration, dried in vacuo, and purified by recrystallization from ethyl acetate (EtOAc) (75 mL) to yield yellow-green crystals (1.8 g, 54%). See, J. Med. Chem., 39:997 (1996).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07179912B2 |
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| 出典データセット | uspto-grants-2007_02 |
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| ORD ID | ord-c5e3e4baf23b4f81ac13c108ef84a414 |
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| 出典メモ | uspto-grants-2007_02 |
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