反应详情

A 2-5 ml microwave vial is charged with Pd(OAc)2 (2.5 mol %, 6.6 mg, 0.0231 mmol), Xantphos (5 mol %, 27.1 mg, 0.0463 mmol), ureido-acetic acid tert-butyl ester (259 mg, 1.482 mmol), and Cs2CO3 (770.2 mg, 2.315 mmol). 3-Bromo-isonicotinic acid methyl ester (216.3 mg, 0.926 mmol) is added, followed by 1,4-dioxane (4 ml). The vessel is sealed and treated in the microwave at 120° C. for 3×3600 seconds. EtOAc is added to the reaction mixture which is then washed with brine (3×20 ml) and water (2×10 ml). The organic phase is passed through Celite® (filter material), dried (MgSO4), filtered and concentrated. The material is purified via flash column chromatography, eluting with iso-hexane:EtOAc to afford the title compound; [M+H]+ 278.

1. customThe vessel is sealed
2. additiontreated in the microwave at 120° C. for 3×3600 seconds
3. washis then washed with brine (3×20 ml) and water (2×10 ml)
4. filtrationThe organic phase is passed through Celite® (filter material)
5. dry with materialdried (MgSO4)
6. filtrationfiltered
7. concentrationconcentrated
8. customThe material is purified via flash column chromatography
9. washeluting with iso-hexane