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3-(Trifluoromethyl)phenol → 4-(3-Trifluoromethylphenoxy)-2-(4-Trifluoromethylphenyl)-Pyrimidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-(Trifluoromethyl)phenol | HCID 7376 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 3,3-Dichloro-2-propenal | HCID 17554 | — |
| 反応物 | 4-Trifluoromethylbenzamidinium acetate | HCID 18541700 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 4-(3-Trifluoromethylphenoxy)-2-(4-Trifluoromethylphenyl)-Pyrimidine | HCID 9929950 | 60% |
反応手順
3-Trifluoromethylphenol (5 mmoles) and subsequently 3,3-dichloroacrolein (5 mmoles) are added to a mixture consisting of a 4-trifluoromethylbenzamidinium acetate (5 mmoles), sodium carbonate (40 mmoles) and acetonitrile (35 ml), which is stirred under reflux. The reaction mixture is stirred for 20 hours under reflux and subsequently cooled down to ambient temperature and filtered through silica. The organic phase is washed with ethyl acetate and concentrated in vacuo. The residue is purified by chromatography on Al2O3 (petrol ethers/ethyl acetate: 2/1) to yield 1.1 g (60%) of the pure product having a melting point of 66-67° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06281358B1 |
| 出典データセット | uspto-grants-2001_08 |
| ORD ID | ord-e641c6794df94fafba17e5482fd781e1 |
| 出典メモ | uspto-grants-2001_08 |