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 (60 mL) was added propylamine (0.7 mL, 8.51 mmol), HATU (1.08 g, 2.84 mmol) and diisopropyl ethyl amine (1.2 mL, 6.9 mmol). The reaction mixture was stirred overnight. The reaction mixture was diluted with CH2Cl2 (50 mL) and water (50 mL) and shaken. 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 1.10 g (84%). LC-MS m/z 484 (M+H)+.

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