関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-(Trifluoromethyl)phenol | HCID 7376 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3,3-Dichloro-2-propenal | HCID 17554 | — |
| 反応物 | 4-Chlorobenzene-1-carboximidamide hydrochloride | HCID 203436 | — |
| 溶媒 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 生成物 | 2-(4-Chlorophenyl)-4-(3-trifluoromethylphenoxy)pyrimidine | HCID 9863254 | 80% |
反応手順
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 4-chlorobenzamidine 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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06559307B2 |
|---|
| 出典データセット | uspto-grants-2003_05 |
|---|
| ORD ID | ord-50784cb5d79444a4869a3c09146eedc7 |
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| 出典メモ | uspto-grants-2003_05 |
|---|
