Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
3-(Trifluoromethyl)phenol → 4-(3-Trifluoromethylphenoxy)-2-(4-Trifluoromethylphenyl)-Pyrimidine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 3-(Trifluoromethyl)phenol | HCID 7376 | — |
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | 3,3-Dichloro-2-propenal | HCID 17554 | — |
| 반응물 | 4-Trifluoromethylbenzamidinium acetate | HCID 18541700 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 4-(3-Trifluoromethylphenoxy)-2-(4-Trifluoromethylphenyl)-Pyrimidine | HCID 9929950 | 60% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06281358B1 |
| 출처 데이터셋 | uspto-grants-2001_08 |
| ORD ID | ord-e641c6794df94fafba17e5482fd781e1 |
| 출처 메모 | uspto-grants-2001_08 |