참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 3-(Trifluoromethyl)phenol | HCID 7376 | — |
| 반응물 | 1,1-Dimethoxyethane | HCID 10795 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 3,3-Dichloro-2-propenal | HCID 17554 | — |
| 반응물 | Cyclopropanecarboximidamide hydrochloride | HCID 2781916 | — |
| 용매 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 생성물 | 2-Cyclopropyl-4-(3-trifluoromethylphenoxy)pyrimidine | HCID 9860497 | 75% |
반응 단계
3,3-Dichloroacrolein (10 mmoles) diluted with dimethoxyethane (35 ml), is slowly added to a mixture consisting of a cyclopropylcarbamidine hydrochloride (10 mmoles), 3-trifluoromethylphenol (11 mmoles), potassium carbonate (40 rnmoles) and dimethyoxyethane (40 ml), which is stirred under reflux. When the addition of 3,3-dichloroacrolein is completed additional cyclopropylcarbamidine 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 2.1 g (75%) of the pure product having as a colorless liquid; 1H NMR (CDC13); δ=2.10 ppm (m, N═C(═N)═CH).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US06559307B2 |
|---|
| 출처 데이터셋 | uspto-grants-2003_05 |
|---|
| ORD ID | ord-1ec957835fbf4ea59e1c911d33f439c8 |
|---|
| 출처 메모 | uspto-grants-2003_05 |
|---|
