反应详情

温度

130 °C

A mixture of methyl 2-amino-3-iodo-5-(trifluoromethyl)benzoate (0.633 g, 1.83 mmoles), trimethylboroxine (0.56 ml, 3.66 mmoles), cesium carbonate (1.2 g, 3.66 mmoles) and 1,1′-bis(diphenylphosphino)ferrocene-palladium(II) dichloride dichloromethane complex (0.075 g, 0.09 mmoles) in 1,4-dioxane (15 mL) was heated in a microwave reactor at 130° C. for 1.5 h. The mixture was partitioned between water (30 ml) and ethyl acetate (2×30 ml). The combined organics were dried over sodium sulphate, filtered and evaporated to dryness. The residue was chromatographed on silica gel eluting with an ethyl acetate/isohexane gradient. This gave the title compound 3 as an orange solid (0.41 g, 96%).

1. customThe mixture was partitioned between water (30 ml) and ethyl acetate (2×30 ml)
2. dry with materialThe combined organics were dried over sodium sulphate
3. filtrationfiltered
4. customevaporated to dryness
5. customThe residue was chromatographed on silica gel eluting with an ethyl acetate/isohexane gradient