反应详情

To the solution of 3-[8-(2,6-difluorophenyl)-2-(methylthio)-7-oxo-5,6,7,8-tetrahydropyrimido[4,5-d]pyrimidin-4-yl]-4-methylbenzoic acid (1.2 g, 2.71 mmol) in CH2Cl2 (80 mL) were added diisopropyl ethyl amine (0.96 mL, 5.5 mmol), HATU (1.044 g, 2.75 mmol) and 4-floroaniline (0.276 mL, 2.92 mmol). The reaction mixture was stirred over night. The reaction mixture was diluted with CH2Cl2 (50 mL) and water (50 mL) and shaked. The layers were separated and the organic layer was washed with brine (75 mL), dried over Na2SO4, filtered and concentrated. CombiFlash chromatography (load column with DCM, mobile phase EtOAc/Hexane) then provided the title compound as a white solid 1.33 g (92%). LC-MS m/z 536 (M+H)+.

1. customThe layers were separated
2. washthe organic layer was washed with brine (75 mL)
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated