反应详情

A solution of 2-chloro-3-nitropyridine (5.0 g, 31.5 mmol), mesitylboric acid (5.65 g, 34.7 mmol), Pd(PPh3)4 (1.82 g, 1.58 mmol) and barium hydroxide octahydrate (14.9 g, 47.3 mmol) in 2,2-dimethoxyethane (150 mL) and water (25 mL) was heated under reflux for one day. 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 chromatogrpahy (10% ethyl acetate/hexane), to give the title compound (5.99 g) as pale yellow oil.

1. temperatureunder reflux for one day
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 chromatogrpahy (10% ethyl acetate/hexane)