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HRID 552027作成日:2026年10月25日

Isopropanol → HCID 21052144、化合物

https://huagongshe.com/reaction/552027

反応式

関与物質

役割名称HCID仕込み量
反応物IsopropanolHCID 3776—
反応物Potassium CarbonateHCID 11430—
反応物(3,4,5-Trifluorophenyl)boronic Acid (contains varying amounts of Anhydride)HCID 2734671—
反応物4-Bromo-3-fluorophenolHCID 2779153—
触媒HCID 178418476HCID 178418476—
溶媒WaterHCID 962—
溶媒TolueneHCID 1140—
生成物HCID 21052144HCID 2105214475.6%

反応条件

温度25 °C

反応手順

4-Bromo-3-fluorophenol (T-10; 5.00 g), 3,4,5-trifluorophenylboronic acid (5.07 g), potassium carbonate (10.9 g), Pd(Ph3P)2Cl2 (0.552 g), and 2-propanol were put in a reaction vessel under a nitrogen atmosphere, and heated under reflux for 5 hours. The reaction mixture was cooled to 25° C., and then poured into water (100 ml) and toluene (100 ml) and mixed. Then, the mixture was allowed to stand to be separated into two layers of organic and aqueous layers, and the extraction to an organic layer was carried out. The obtained organic layer was fractionated, washed with water, and then dried over anhydrous magnesium sulfate. The obtained solution was concentrated under reduced pressure, and the residue was purified with a fractional operation by means of column chromatography using toluene as the eluent and silica gel as the stationary phase powder. The product was further purified by recrystallization from a mixed solvent of heptane/Solmix A-11 and dried, whereby 4.79 g of 4-hydroxy-2,3′,4′,5′-tetrafluoro-1,1′-biphenyl (T-11) was obtained. The yield based on the compound (T-1) was 74%.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07951433B2
出典データセットuspto-grants-2011_05
ORD IDord-1e59d64b25214a84b3fd707f1ef8c6c0
出典メモuspto-grants-2011_05