反应详情

A suspension of 1-(2-(2-(2,5-dichloropyrimidin-4-yl)ethyl)phenyl)cyclopropanecarboxamide A14 (0.150 g, 0.446 mmol), Cs2CO3 (436 mg, 1.34 mmol) and 2-aminoxazole (75.0 mg, 0.892 mmol) in 1,4-dioxane (3 mL) was sonicated for 10 minutes. Xantphos (10 mg, 18 μmol) and Pd(II) acetate (2.0 mg, 8.9 μmol) were added and the reaction was irradiated in the microwave for 20 minutes at 120° C. The resulting mixture was adsorbed onto silica gel and purified by column chromatography (Biotage Isolera, 24 g SiO2 cartridge, 0-100% EtOAc in cyclohexane then 0-20% MeOH in EtOAc) to give a solid. Acetone (0.5 mL) followed by cyclohexane (25 mL) was added and the mixture was sonicated for 10 minutes. The resulting precipitate was collected by filtration and the filter cake was washed with cyclohexane (25 mL) and dried under high vacuum to give the title compound 11 as a white solid (10 mg, 6%). LCMS-B: rt 4.64 min; m/z 384.0 [M+H]+.

1. customwas sonicated for 10 minutes
2. customthe reaction was irradiated in the microwave for 20 minutes at 120° C
3. custompurified by column chromatography (Biotage Isolera, 24 g SiO2 cartridge, 0-100% EtOAc in cyclohexane
4. custom0-20% MeOH in EtOAc) to give a solid
5. additionwas added
6. customthe mixture was sonicated for 10 minutes
7. filtrationThe resulting precipitate was collected by filtration
8. washthe filter cake was washed with cyclohexane (25 mL)
9. customdried under high vacuum