反应详情

In a sealed tube under nitrogen was placed 4-amino-N-hydroxy-6-(methyl-3-methylphenyl-amino)-[1,3,5]triazine-2-carboxamidine (Intermediate 1, 100 mg, 380 μmol). Then 5 mL anhydrous pyridine was added followed by 6-(2,2,2-trifluoroethoxy)-nicotinoyl chloride (prepared in an analogous manner to Intermediate 57, 91 mg, 380 μmol). The mixture was stirred at room temperature for 48 hrs. After this time the mixture was heated at 115 C for 18 h, allowed to cool and concentrated in vacuo. The crude residue was loaded onto a 2 g isolute silica column in a minimal amount of DCM and eluted with ethyl acetate-heptane 20-50% to give the title compound (54 mg, 32%).

1. customIn a sealed tube under nitrogen was placed
2. temperatureAfter this time the mixture was heated at 115 C for 18 h
3. temperatureto cool
4. concentrationconcentrated in vacuo
5. washeluted with ethyl acetate-heptane 20-50%