반응 #69529

반응 방정식

1-bromo-3,5-dimethoxybenzene

2-dicyclohexylphosphino-2′,6′-dimethoxybiphenyl

cesium carbonate

→

title compound

1-Cyclopropyl-3,5-dimethoxybenzene

용매

water

dioxane

water

반응 조건

후처리

1. 1
   추출was extracted with ethyl acetate
2. 2
   건조dried over anhydrous magnesium sulfate
3. 3
   workup.DISTILLATIONthe solvent was distilled off under reduced pressure
4. 4
   기타The residue was purified by silica gel column chromatography (n-heptane/ethyl acetate: 3/1)

실험 절차

To a solution of 1-bromo-3,5-dimethoxybenzene (2.00 g, 9.21 mmol) in dioxane (30 mL) and water (10 mL) were added potassium cyclopropyl trifluoroborate (2.73 g, 18.4 mmol), 2-dicyclohexylphosphino-2′,6′-dimethoxybiphenyl (756 mg, 1.84 mmol), palladium(II) acetate (207 mg, 0.92 mmol) and cesium carbonate (18.0 g, 55.3 mmol), and the mixture was heated at 100° C. for 16 hours. After the reaction was completed, water was added to the reaction mixture, which was extracted with ethyl acetate and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (n-heptane/ethyl acetate: 3/1) to obtain the title compound (1.61 g, 9.03 mmol).

출처