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-Chlorobenzene-1-carboximidamide hydrochloride | HCID 203436 | — |
| 용매 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 생성물 | 2-(4-Chlorophenyl)-4-(3-trifluoromethylphenoxy)pyrimidine | HCID 9863254 | 80% |
반응 단계
3,3-Dichloroacrolein (10 mmoles) diluted with dimethoxyethane (35 ml), is slowly added to a mixture consisting of a 4-chlorobenzamidine hydrochloride (10 mmoles), 3-trifluoromethylphenol (11 mmoles), potassium carbonate (40 mmoles) and dimethoxyethane (40 ml), which is stirred under reflux. When the addition of 3,3-dichloroacrolein is completed additional 4chlorobenzamidine hydrochloride (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 2.79 g (80%) of the pure product having a melting point of 92° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US06281358B1 |
|---|
| 출처 데이터셋 | uspto-grants-2001_08 |
|---|
| ORD ID | ord-f768b74fdf1545feb0499b9dc0950bd9 |
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| 출처 메모 | uspto-grants-2001_08 |
|---|
