反应详情

温度

80 °C

A mixture of N-[3-bromo-6-(methyloxy)-2-pyridinyl]-2,2-dimethylpropanamide (78.738 g, 274 mmol), bis(tri-t-butylphosphine)palladium(0) (1 g, 1.957 mmol) and tris(dibenzylideneacetone)dipalladium(0) (0.892 g, 0.974 mmol) in dry, degassed 1,4-dioxane (600 ml) was treated with n-butyl acrylate (47.1 ml, 329 mmol) and dicyclohexylmethylamine (64.5 ml, 302 mmol). The reaction mixture was then heated at 80° C. for 4 h and then at 120° C. for 3 h. The reaction was then evaporated and water (1000 ml) was added and the mixture was extracted with Et2O (3×500 ml). The combined organic solvents were then dried (MgSO4), filtered, evaporated to give the crude product. This was then dissolved in DCM (300 ml) and chromatographed (10-30% EtOAc:40-60 petroleum ether) and then dried in vacuo to give product as a white solid (87.412 g, 95%).

1. customin dry
2. customdegassed 1,4-dioxane (600 ml)
3. customThe reaction was then evaporated
4. additionwater (1000 ml) was added
5. extractionthe mixture was extracted with Et2O (3×500 ml)
6. dry with materialThe combined organic solvents were then dried (MgSO4)
7. filtrationfiltered
8. customevaporated
9. customto give the crude product
10. customchromatographed (10-30% EtOAc:40-60 petroleum ether)
11. customdried in vacuo