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HRID 914827作成日:2026年10月27日

Hydrochloric Acid → 2-(4-Fluoro-3-thienyl)-1-(4-pyridyl)ethanone

https://huagongshe.com/reaction/914827

反応式

関与物質

役割名称HCID仕込み量
反応物Hydrochloric AcidHCID 313—
反応物Cesium carbonateHCID 10796—
反応物Sodium HydroxideHCID 14798—
反応物Diphenyl (phenylamino)(pyridin-4-yl)methylphosphonateHCID 423769—
反応物4-Fluorothiophene-3-carbaldehydeHCID 22247846—
溶媒2-Furanpropanol, tetrahydro-HCID 13020—
生成物2-(4-Fluoro-3-thienyl)-1-(4-pyridyl)ethanoneHCID 2224802036%

反応手順

After dissolving 19.6 g of [(phenylamino)-(4-pyridylmethyl)]phosphonic acid diphenyl ester [CAS No. 3360-72-3] in 115 ml of tetrahydrofuran-2-propanol (4:1), 6.02 g of 4-fluorothiophene-3-carboxaldehyde and 19.61 g of anhydrous cesium carbonate were added and the mixture was stirred overnight at room temperature. Next, 90 ml of 5N hydrochloric acid was added to the reaction mixture and the mixture was stirred at room temperature for 6 hours. After adding a 5N sodium hydroxide solution to the reaction solution, extraction was performed with ethyl acetate. The organic layer was washed with water and saturated brine and dried over anhydrous magnesium sulfate, and then the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (solvent: n-hexane/ethyl acetate). The obtained solid was washed with n-hexane to obtain the title compound (3.66 g, 36% yield).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07265108B2
出典データセットuspto-grants-2007_09
ORD IDord-9da64ea8e8ed453aa3c20cca7b286d84
出典メモuspto-grants-2007_09