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
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
To a stirred solution of 1-benzenesulfonyl-4-(4-bromo-phenyl)-3-phenyl-imidazolidin-2-one (100 mg) and 4-carboxyphenylboronic acid (57 mg) in dioxane (0.6 mL) and water (0.4 mL) under argon were added a 2 M aqueous sodium carbonate solution (0.33 mL) and dichloro[1,1′-bis(diphenylphosphino)ferrocene]palladium dichloromethane adduct (9 mg). The mixture was stirred at 80° C. for 3 h. After cooling to room temperature, the mixture was filtered. The filtrate was diluted with ethyl acetate and washed with 10% aqueous KHSO4 solution. The org. phase was dried (MgSO4), filtered and concentrated. The product was purified using column chromatography (SiO2, dichloromethane/methanol 1:0=>4:1) to give 4′-(1-benzenesulfonyl-2-oxo-3-phenyl-imidazolidin-4-yl)-biphenyl-4-carboxylic acid (36 mg) as an off-white solid. MS: 497.1 ([M−H]−)
WORKUP
后处理
- temperatureAfter cooling to room temperature
- filtrationthe mixture was filtered
- additionThe filtrate was diluted with ethyl acetate
- washwashed with 10% aqueous KHSO4 solution
- dry with materialphase was dried (MgSO4)
- filtrationfiltered
- concentrationconcentrated
- customThe product was purified