関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Methylpiperazine | HCID 53167 | — |
| 反応物 | 1-(5-Chloro-2-nitrophenyl)piperidine | HCID 3096079 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-Methyl-4-(4-nitro-3-(piperidin-1-yl)phenyl)piperazine | HCID 2885704 | 99% |
反応手順
A mixture of 350 mg (1.45 mmol) of 1-(5-chloro-2-nitro-phenyl)-piperidine (as prepared in Example 4, step (a)) and 482 μL (4.35 mmol) of 1-methylpiperazine was heated in a sealed vial at 138° C. for 30 h. The mixture was cooled and poured into 60 mL of water and extracted with EtOAc (2×20 mL). The combined extracts were washed with brine (30 mL), dried (Na2SO4) and concentrated in vacuo to afford 436 mg (99%) of the title compound as a yellow resin: Mass spectrum (ESI, m/z): Calcd. for C16H24N4O2, 305.2 (M+H), found 305.2.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07705042B2 |
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| 出典データセット | uspto-grants-2010_04 |
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| ORD ID | ord-552f2b9daed04d169512e287fe23c668 |
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| 出典メモ | uspto-grants-2010_04 |
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