참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 3-(Trifluoromethyl)phenol | HCID 7376 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 3,3-Dichloro-2-propenal | HCID 17554 | — |
| 반응물 | 4-Fluorobenzamidine acetate | HCID 44784991 | — |
| 용매 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 생성물 | 4-(3-Trifluoromethylphenoxy)-2-(4-fluorophenyl)pyrimidine | HCID 9862497 | 75.4% |
반응 단계
3,3-Dichloroacrolein (10 mmoles) diluted with dimethoxyethane (35 ml), is slowly added to a mixture consisting of a 4-fluorobenzamidine acetate (10 mmoles), 3-trifluoromethylphenol (11 mmoles), potassium carbonate (40 mmoles) nd dimethoxyethane (40 ml), which is stirred under reflux. When the addition of 3,3-dichloroacrolein is completed additional 4-fluorobenzamidine acetate (1 mmoles) is added. The reaction mixture is stirred for 3 hours under reflux and subsequently cooled down to ambient temperature over night and filtered through silica. The organic phase is concentrated in vacuo. The residue was purified by chromatography on Al2O3 (petrol ethers/ethyl acetate: 20/1) to yield 2.52 g (75%) of the pure product having a melting point of 52° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US06559307B2 |
|---|
| 출처 데이터셋 | uspto-grants-2003_05 |
|---|
| ORD ID | ord-e7c4df2732b2437d9a887a4aae508376 |
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| 출처 메모 | uspto-grants-2003_05 |
|---|
