関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitromethane | HCID 6375 | — |
| 反応物 | Ammonium Acetate | HCID 517165 | — |
| 反応物 | 5-(3,4-Dichlorophenyl)-2-furaldehyde | HCID 617688 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | (E)-2-(5-(3,4-dichlorophenyl)furan-2-yl)ethenamine | HCID 67170044 | 92.5% |
反応手順
To a stirred solution of 5-(3,4-dichlorophenyl)furfural (1.18 g, 4.89 mmol) in acetic acid (30 ml) was added nitromethane (0.535 ml, 9.78 mmol) and ammonium acetate (1.13 g, 14.7 mmol). The reaction mixture was heated at 80° C. for 4.5 h. Cooled reaction mixture was poured onto ice water (30 ml) and thus formed precipitate was filtered, washed with water and dried under vacuum to give 1.15 g (83%) of the title compound. 1H-NMR (400 MHz; d6-DMSO): δ 7.37 (d, 1H), 7.43 (d, 1H), 7.76 (d, 1H), 7.95 (dd, 1H), 8.03 (d, 1H), 8.19 (d, 1H), 8.31 (d, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08975254B2 |
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| 出典データセット | uspto-grants-2015_03 |
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| ORD ID | ord-d3ec8c8042a2450380a5863f5cd8d24d |
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| 出典メモ | uspto-grants-2015_03 |
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