反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
0.34 g of 4-bromo-2-fluorobenzonitrile, 1.4 g of caesium carbonate, 0.08 g of (9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphane) and 25 mg of palladium acetate are successively added, under argon, to a solution of 0.31 g of [5-(9H-carbazol-4-yl)pyridin-2-yl]methanol in 15 ml of dioxane. The reaction mixture is refluxed for 4 hours, cooled to ambient temperature, filtered through celite and concentrated under reduced pressure. The residue is purified by silica gel chromatography, elution being carried out with a mixture of cyclohexane and ethyl acetate (85/15 by volume), so as to give 70 mg of 2-fluoro-4-{4-[6-(hydroxymethyl)pyridin-3-yl]-9H-carbazol-9-yl}benzonitrile in the form of a yellow solid, the characteristics of which are the following:
WORKUP
后处理
- temperatureThe reaction mixture is refluxed for 4 hours
- filtrationfiltered through celite and
- concentrationconcentrated under reduced pressure
- customThe residue is purified by silica gel chromatography, elution
- additionbeing carried out with a mixture of cyclohexane and ethyl acetate (85/15 by volume)