참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | 3-(Trifluoromethyl)phenol | HCID 7376 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 3,3-Dichloro-2-propenal | HCID 17554 | — |
| 반응물 | 1,1,1,3-Tetrachloro-3-ethoxypropane | HCID 12350822 | — |
| 반응물 | 4-(Trifluoromethyl)benzamidine Hydrochloride | HCID 12535791 | — |
| 용매 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 생성물 | 4-(3-Trifluoromethylphenoxy)-2-(4-Trifluoromethylphenyl)-Pyrimidine | HCID 9929950 | 80% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06281358B1 |
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| 출처 데이터셋 | uspto-grants-2001_08 |
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| ORD ID | ord-3a1cc3098a754159b141577cb43d17d3 |
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| 출처 메모 | uspto-grants-2001_08 |
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