反应详情

温度

160 °C

To a mixture of 2-(5-bromo-2-cyclopropylphenyl)cyclopentane-1,3-dione (0.100 g, 0.34 mmol), 2,4-dichlorophenylboronic acid (0.090 g, 0.47 mmol), [1,1′-bis(diphenylphosphino)-ferrocene]palladium(II)chloride (22 mg, 0.027 mmol) and cesium fluoride (0.152 g, 1.0 mmol) is added 1,2-dimethoxyethane (1 ml). After evacuating and flushing with nitrogen (×3) the mixture is heated at 160° C. for 15 minutes under microwave irradiation. After dilution with distilled water the crude product is extracted with ethyl acetate (×3), and the organic phase is washed with brine, dried over magnesium sulfate and concentrated in vacuo. The crude product is then purified by flash column chromatography on silica gel (isohexane/ethyl acetate eluant) and further triturated with hexanes to afford 2-(2′,4′-dichloro-4-cyclopropylbiphenyl-3-yl)-cyclopentane-1,3-dione as a white powder.

1. customAfter evacuating
2. customflushing with nitrogen (×3) the mixture
3. extractionAfter dilution with distilled water the crude product is extracted with ethyl acetate (×3)
4. washthe organic phase is washed with brine
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated in vacuo
7. customThe crude product is then purified by flash column chromatography on silica gel (isohexane/ethyl acetate eluant)
8. customfurther triturated with hexanes