関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | p-Fluoronitrobenzene | HCID 9590 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | N,N-Dimethyl-1,4-cyclohexanediamine | HCID 345823 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | N1,N1-dimethyl-N4-(4-nitrophenyl)cyclohexane-1,4-diamine | HCID 86681775 | — |
反応手順
To a solution of 1-fluoro-4-nitrobenzene (0.392 ml, 3.69 mmol) in 4 mL of dimethyl sulfoxide was added N1,N1-dimethylcyclohexane-1,4-diamine (500 mg, 3.52 mmol) and N-ethyl-N-isopropylpropan-2-amine (2.449 ml, 14.06 mmol). The reaction mixture was stirred at 100° C. for 24 hours. The mixture was poured into a separatory funnel and was diluted with 50 mL of ethyl acetate. The organic mixture was then washed with 50 mL of water followed by 50 mL of saturated aqueous brine. The organic phase was dried over sodium sulfate, filtered and concentrated. The crude material obtained was carried through the next step without purification. MS (ESI) m/z 264.1 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09181239B2 |
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| 出典データセット | uspto-grants-2015_11 |
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| ORD ID | ord-81b1736b12654061a6b28cc9c4969376 |
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| 出典メモ | uspto-grants-2015_11 |
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