反应详情

温度

110 °C

A mixture of 330 mg (1.625 mmol) 3-bromo-6-methoxy-pyridin-2-yl-amine, 396 mg (3.25 mmol) phenylboronic acid, 1 ml 2N Na2CO3 and 59 mg (0.08 mmol) dichloro[1,1′-bis(diphenylphosphino)-ferrocene]palladium (II) dichloromethane adduct in 10 ml dioxane was heated to 110° C. for 2 h. The mixture was concentrated, diluted Na2CO3 aq. was added and extracted 2× with 100 ml diethyl ether. The combined organic phases were dried with MgSO4 and evaporated. The residue was purified by flash column chromatography on silica-eluting with a gradient of hexane/ethyl acetate to yield 230 mg (71%) of the title compound.

1. concentrationThe mixture was concentrated
2. additiondiluted Na2CO3 aq. was added
3. extractionextracted 2× with 100 ml diethyl ether
4. dry with materialThe combined organic phases were dried with MgSO4
5. customevaporated
6. customThe residue was purified by flash column chromatography on silica-
7. washeluting with a gradient of hexane/ethyl acetate