反应详情

[4-(2-Chloro-pyridin-3-yl)-[1,3,5]triazin-2-yl]-(3,4,5-trimethoxy-phenyl)amine (Example 2, Step 4) (247 mg, 1.08 mmol) was suspended in a 2 M solution of NH3 in IpOH (3 ml)(Aldrich), and the reaction mixture was stirred overnight in a sealed tube. Concentration, trituration in a small amount of MeOH, and filtration provided a white solid. A portion of this material (97 mg, 0.47 mmol) was mixed with 3-amino-N-(4-phenoxyphenyl)benzamide (320 mg, 0.96 mmol) and DMSO (250 ml), and stirred overnight at 90° C. The dark residue was diluted with IpOH, sonicated, triturated, and then concentrated. Upon dilution with IpOH, a light green solid was isolated by filtration. MS m/z=476.5. [M+H]+. Calc'd for C27H21N7O2: 475.18.

1. concentrationConcentration, trituration
2. filtrationin a small amount of MeOH, and filtration
3. customprovided a white solid
4. stirringstirred overnight at 90° C
5. additionThe dark residue was diluted with IpOH
6. customsonicated
7. customtriturated
8. concentrationconcentrated
9. customUpon dilution with IpOH, a light green solid was isolated by filtration