反应详情

A mixture of 6-chloro-N-(3-iodo-4-methyl-phenyl)-nicotinamide (50 mg, 0.13 mmol) and morpholine (35 mg, 0.42 mmol), diisopropylethyl amine (0.07 mL, 0.42 mmol) and a catalytic amount of DMAP in dioxane (5 mL) was heated at 120° C. in a sealed tube until consumption of the limiting reagent. The mixture was then cooled and partitioned between EtOAc and water. Organic layer was removed, dried over Na2SO4 filtered and concentrated to a residue that after a silica gel column with 20-40% EtOAc in hexanes gradient afforded the product. HRMS m/z calcd for C17H18N3O2I [M+H]+: 424.0517. Found: 424.0516.

1. temperatureThe mixture was then cooled
2. custompartitioned between EtOAc and water
3. customOrganic layer was removed
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated to a residue that after a silica gel column with 20-40% EtOAc in hexanes gradient
7. customafforded the product