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Ethanol → 5-Bromo-2-(tetrahydropyran-4-yl)nitrobenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-Aminotetrahydropyran | HCID 419223 | — |
| 反応物 | 4-Bromo-1-fluoro-2-nitrobenzene | HCID 2736328 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5-Bromo-2-(tetrahydropyran-4-yl)nitrobenzene | HCID 67498826 | 91.2% |
反応手順
An eggplant flask was charged with 5-bromo-2-fluoronitrobenzene (3.0 g, 13.6 mmol), triethylamine (1.66 g, 16.3 mmol), 4-aminotetrahydropyran (1.52 g, 15.0 mmol), and ethanol (60 mL), and this was heated to reflux with stirring for 2 hours. After concentration of the reaction mixture under reduced pressure, water (60 mL) was added and this was stirred as is at room temperature for 30 minutes. The precipitated crystals were filtered off and washed with water. The crystals obtained were dried at reduced pressure with heating to yield the title compound (3.55 g, 86% yield) as a reddish-orange solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08829035B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-3a8229f9c17741f3846e907f5ce44fc5 |
| 出典メモ | uspto-grants-2014_09 |