反应详情

Intermediate 1 (228 mg) obtained in Example 1, Step A is added with phenylboronic acid (122 mg, Aldrich), tetrakis(triphenylphosphine)palladium(0) (116 mg), 1,2-dimethoxyethane (5 ml) and 2 N aqueous sodium carbonate (2 ml), and the mixture is refluxed by heating for 5 hours under a nitrogen gas atmosphere. The reaction mixture is cooled to room temperature, then added with water (25 ml), and extracted 3 times with ethyl acetate (20 ml for each time), and the combined organic layer is washed with saturated brine (30 ml), and dried over anhydrous magnesium sulfate. The solvent is evaporated under reduced pressure, and the residue is purified by silica gel chromatography (n-hexane:ethyl acetate=2:1) to obtain the title compound (158 mg (predictive yield)).

1. temperaturethe mixture is refluxed
2. temperatureby heating for 5 hours under a nitrogen gas atmosphere
3. extractionextracted 3 times with ethyl acetate (20 ml for each time), and the combined organic layer
4. washis washed with saturated brine (30 ml)
5. dry with materialdried over anhydrous magnesium sulfate
6. customThe solvent is evaporated under reduced pressure
7. customthe residue is purified by silica gel chromatography (n-hexane:ethyl acetate=2:1)