反应详情

0.21 g of dichlorobis(tricyclohexylphosphine)palladium, 0.66 g of 3-pyridyl-boronic acid and 14 ml of a 2N sodium carbonate solution are added to a solution of 1.02 g of 2-amino-5-bromo-3-nitropyridine in 40 ml of degassed dioxane. The mixture is heated to reflux under N2 for 28 hours and, after cooling and addition of water, extracted three times with dichloromethane. The combined organic phases are dried over sodium sulfate, concentrated and the residue is crystallized from ethyl acetate. This gives 0.58 g of the title compound of m.p. 226–228° C. The mass spectrum shows the molecular peak MH+ at 217.2 Da.

1. temperatureThe mixture is heated
2. temperatureto reflux under N2 for 28 hours
3. temperatureafter cooling
4. extractionextracted three times with dichloromethane
5. dry with materialThe combined organic phases are dried over sodium sulfate
6. concentrationconcentrated
7. customthe residue is crystallized from ethyl acetate