反应详情

3-[8-(2,6-Difluorophenyl)-2-(methylsulfinyl)-7-oxo-7,8-dihydropyrido[2,3-d]pyrimidin-4-yl]-4-methyl-N-(phenylmethyl)benzamide (0.084 g, 0.154 mmol) and (1H-imidazol-2-ylmethyl)amine dihydrochloride (0.039 g, 0.23 mmol) were dissolved in CH2Cl2 (5 mL) and triethylamine (0.7 mL). The resulting mixture was stirred under argon at room temperature overnight. The solvents were pumped off in vacuo, and the residue taken up in EtOAc and 1 N NaOH. The organic phase was washed with brine, dried over anhydrous Na2SO4 filtered and evaporated. The residue was flash chromatographed on silica gel (20 g) eluted with 6:1:0.05 CH2Cl2:isopropanol:NH4OH. The material isolated was not pure, and was rechromatographed on silica gel (20 g) eluted with 0-5% MeOH/CH2Cl2 to give the title compound as a white amorphous solid. mp (dec) 185-190° C. LC-MS m/z 578 (M+H)+, 1.76 min (ret time).

1. washThe organic phase was washed with brine
2. dry with materialdried over anhydrous Na2SO4
3. filtrationfiltered
4. customevaporated
5. customchromatographed on silica gel (20 g)
6. washeluted with 6:1:0.05 CH2Cl2
7. customThe material isolated
8. customwas rechromatographed on silica gel (20 g)
9. washeluted with 0-5% MeOH/CH2Cl2