反应详情

According to the method of Preparation 25(a), 2-bromo-5-nitrotoluene (15 gm, 69.4 mmol) was treated with phenyl boronic acid (12.7 gm, 104.1 mmol) under palladium catalysis, using 2M aqueous sodium carbonate as base at reflux in dimethoxyethane for 16 h. After being cooled, the mixture was separated the organic layer was diluted with diethyl ether and washed with water (twice). The organic layer was dried (Na2SO4) and concentrated under reduced pressure. The residue was purified by flash chromatography (gradient elution with hexane to hexane:ethyl acetate 95:5) to give 2-methyl-4-nitro-1-phenylbenzene as a yellow solid (12.7gm, 86%).

1. temperatureAfter being cooled
2. customthe mixture was separated the organic layer
3. additionwas diluted with diethyl ether
4. washwashed with water (twice)
5. dry with materialThe organic layer was dried (Na2SO4)
6. concentrationconcentrated under reduced pressure
7. customThe residue was purified by flash chromatography (gradient elution with hexane to hexane:ethyl acetate 95:5)