関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Bromo-4-nitrobenzene | HCID 11466 | — |
| 反応物 | 1-Ethylpiperazine | HCID 79196 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane methanol | HCID 21226129 | — |
| 生成物 | 1-Ethyl-4-(4-nitrophenyl)piperazine | HCID 2857549 | — |
反応手順
A mixture of 1-bromo-4-nitrobenzene (6 g, 29.7 mmol) and 1-ethylpiperazine (7.6 mL, 59.4 mmol, 2 equiv) is heated to 80° C. for 15 h. After cooling to RT, the reaction mixture is diluted with water and DCM/MeOH, 9:1. The aqueous layer is separated and extracted with DCM/MeOH, 9:1. The organic phase is washed with brine, dried (sodium sulfate), filtered and concentrated. Purification of the residue by silica gel column chromatography (DCM/MeOH+1% NH3aq, 9:1) affords the title compound as a yellow solid: ESI-MS: 236.0 [MH]+; tR=2.35 min (purity: 100%, system 1); TLC: Rf=0.50 (DCM/MeOH+1% NH3aq, 9:1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08759517B2 |
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| 出典データセット | uspto-grants-2014_06 |
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| ORD ID | ord-f404d9e1f79343e5b53672e82eea05b4 |
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| 出典メモ | uspto-grants-2014_06 |
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