反应详情

温度

80 °C

A mixture of 2,4-dimethoxyphenylboronic acid (25.0 g, 137 mmol), methyl 2-bromo-5-nitrobenzoate (35.7 g, 137 mmol), cesium carbonate (89.4 g, 274 mmol) and bis(triphenylphosphine)palladium (II) dichloride (4.81 g, 6.85 mmol) was suspended in N,N-dimethylformamide (450 mL), and then the suspension was stirred under argon atmosphere at 80° C. overnight. After cooling down, ethyl acetate (200 mL), diethylether (400 mL) and water (1000 mL) were added thereto and the mixture was separated into a water phase and an organic layer. The water layer was extracted with a mixed solvent of ethyl acetate (150 mL)-diethylether (150 mL) (twice). The combined organic layer was washed with water (500 mL, 3 times) and saturated brine (500 mL) successively, dried over anhydrous magnesium sulfate, and then the solvent was removed under reduced pressure to give the titled reference compound as a brown oil. (Quantitative)

1. temperatureAfter cooling down
2. customthe mixture was separated into a water phase
3. extractionThe water layer was extracted with a mixed solvent of ethyl acetate (150 mL)-diethylether (150 mL) (twice)
4. washThe combined organic layer was washed with water (500 mL, 3 times) and saturated brine (500 mL) successively
5. dry with materialdried over anhydrous magnesium sulfate
6. customthe solvent was removed under reduced pressure
7. customto give the titled reference compound as a brown oil