反应详情

A solution of 2-bromo-6-nitrotoluene (10.0 g, 46 mmol), mesitylboric acid (8.3 g, 51 mmol), Pd(PPh3)4 (2.7 g, 2.31 mmol) and barium hydroxide octahydrate (21.9 g, 69 mmol) in 2,2-dimethoxyethane (300 mL) and water (50 mL) was heated under reflux for six hours. The mixture was filtered through Celite, and the filtrate was diluted with ethyl acetate, washed with brine, dried over anhydrous magnesium sulfate and evaporated. The residue was purified by silica gel column chromatography (0-1% ethyl acetate/hexane), to give the title compound (11.0 g) as white crystals.

1. temperatureunder reflux for six hours
2. filtrationThe mixture was filtered through Celite
3. additionthe filtrate was diluted with ethyl acetate
4. washwashed with brine
5. dry with materialdried over anhydrous magnesium sulfate
6. customevaporated
7. customThe residue was purified by silica gel column chromatography (0-1% ethyl acetate/hexane)