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HRID 1943513作成日:2026年10月23日

Sodium Carbonate → 2-(4'-Ethyl-3-fluorobiphenyl-4-yl)-5-methylthiophene

https://huagongshe.com/ja/reaction/1943513

反応式

関与物質

役割名称HCID仕込み量
反応物Sodium CarbonateHCID 10340—
反応物2-Bromo-5-methylthiopheneHCID 69831—
反応物4'-Ethyl-3-fluorobiphenyl-4-boronic acidHCID 53402575—
触媒HCID 178418397HCID 178418397—
溶媒Toluene ethanolHCID 21863594—
生成物2-(4'-Ethyl-3-fluorobiphenyl-4-yl)-5-methylthiopheneHCID 58160695—

反応手順

A mixture of 5.0 g (28.2 mmol) of 2-bromo-5-methylthiophene, 7.70 g (28.3 mmol) of 4′-ethyl-3-fluoro-4-biphenylboronic acid, 1.70 g (1.47 mmol) of tetrakis(triphenylphosphine)palladium(0) and 30 ml of 2 N sodium carbonate solution in 90 ml of toluene/ethanol (1:2) is refluxed for 3 h. After cooling, the organic phase is separated off, and the aqueous phase is extracted a number of times with toluene. The combined organic phases are washed with water and sat. sodium chloride solution. The solution is dried using sodium sulfate and evaporated to dryness. The residue is purified by column chromatography (SiO2, n-heptane:toluene=97:3). The further purification is carried out by recrystallisation from ethanol and n-heptane, giving 2-(4′-ethyl-3-fluorobiphenyl-4-yl)-5-methylthiophene as a colourless solid (m.p. 102° C.).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08394293B2
出典データセットuspto-grants-2013_03
ORD IDord-05f7bf8fa6664e07a70360f0b33c850a
出典メモuspto-grants-2013_03