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HRID 253702作成日:2026年10月26日

Tripropylamine → 4-Chloro-6-methyl-2-(2-trifluoromethyl-phenyl)-pyrimidine

https://huagongshe.com/reaction/253702

反応式

関与物質

役割名称HCID仕込み量
反応物TripropylamineHCID 7616—
反応物Phosphorus oxychlorideHCID 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)-pyrimidineHCID 2193927184.1%

反応条件

温度115 °C

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

DOI10.6084/m9.figshare.5104873.v1
特許番号US07872129B2
出典データセットuspto-grants-2011_01
ORD IDord-9bdff50eafca4cbbb0601d2dc0730ab9
出典メモuspto-grants-2011_01