反应详情

A mixture of 4-bromo-3-fluoroanisole, 2-methylphenyl boronic acid, tetrakis(triphenylphosphine) palladium (5% mol) and sodium carbonate (0.23 g, 2.1 mmol) in 20 ml of water/EtOH/toluene (1:2:4) was heated to reflux for 5 h. TLC (EtOAc:hexane/2:98) showed that the reaction was over. The solvents was removed. Water (10 ml) was added. The organic was extracted with methylene chloride (3×50 ml). The combined methylene chloride layers were washed with brine, and dried over sodium sulfate. The title compound was obtained after purification with preparative TLC using 2% EtOAc in hexane as the eluant.

1. temperaturewas heated
2. temperatureto reflux for 5 h
3. customThe solvents was removed
4. additionWater (10 ml) was added
5. extractionThe organic was extracted with methylene chloride (3×50 ml)
6. washThe combined methylene chloride layers were washed with brine
7. dry with materialdried over sodium sulfate