関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tripropylamine | HCID 7616 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | 4(3H)-Pyrimidinone, 6-methyl-2-[2-(trifluoromethyl)phenyl]- | HCID 135850835 | — |
| 生成物 | 4-Chloro-6-methyl-2-(2-trifluoromethyl-phenyl)-pyrimidine | HCID 21939271 | 84.1% |
反応手順
A solution of 6-methyl-2-(2-trifluoromethyl-phenyl)-3H-pyrimidin-4-one (10.7 g, 41.9 mmol) in phosphorous oxychloride (39 mL, 419 mmol) was treated with tri-n-propylamine (16 mL, 83.9 mmol) and refluxed at 110-120° C. for 1 hours. The solvent was evaporated, azeotroped three times with toluene, then dried in vacuo. The residue was taken up in ethyl acetate, washed sequentially with 1 N sodium hydroxide, water and brine, then dried over sodium sulfate and concentrated. Purification by flash chromatography [SiO2, ethyl acetate:hexanes (1:9)] provided the title compound (9.61 g, 84% yield) as an orange oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07872129B2 |
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| 出典データセット | uspto-grants-2011_01 |
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| ORD ID | ord-9bdff50eafca4cbbb0601d2dc0730ab9 |
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| 出典メモ | uspto-grants-2011_01 |
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