関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 3-(Trifluoromethyl)phenol | HCID 7376 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3,3-Dichloro-2-propenal | HCID 17554 | — |
| 反応物 | 1,1,1,3-Tetrachloro-3-ethoxypropane | HCID 12350822 | — |
| 反応物 | 4-(Trifluoromethyl)benzamidine Hydrochloride | HCID 12535791 | — |
| 溶媒 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 生成物 | 4-(3-Trifluoromethylphenoxy)-2-(4-Trifluoromethylphenyl)-Pyrimidine | HCID 9929950 | 80% |
反応手順
Water (20 mmoles) is added to a solution of 1,1,1,3-tetrachloro-3-ethoxypropane (10 mmoles) in dimethoxyethane (25 ml). The reaction mixture is stirred for 2 h under reflux. The resulting mixture is slowly added to a mixture consisting of a 4-trifluoromethylbenzamidine hydrochloride (10 mmoles), 3-trifluoromethylphenol (11 mmoles), potassium carbonate (60 mmoles) and dimethoxyethane (50 ml), which is stirred under reflux. When the addition of 3,3-dichloroacrolein solution is completed additional 4-trifluoromethylbenzamidine hydrochloride (1 mmoles) is added. The reaction mixture is stirred for 2 hours under reflux and subsequently cooled down to ambient temperature, filtered through silica, and the organic phase is concentrated in vacuo. The residue is purified by chromatography on SiO2 (petrol ethers/diisopropylether: 6/1) to yield 3,07 g (80%) of the product having a melting point of 66-67° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06281358B1 |
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| 出典データセット | uspto-grants-2001_08 |
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| ORD ID | ord-3a1cc3098a754159b141577cb43d17d3 |
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| 出典メモ | uspto-grants-2001_08 |
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