反应详情

温度

90 °C

7-ethyl-2-(2-(4-fluorophenyl)-1H-imidazol-1-yl)-5-methyl-8-(1H-pyrazol-4-yl)-7,8-dihydropteridin-6(5H)-one (Example 331, 55 mg, 0.131 mmol) was dissolved in 3 mL of dioxane and Me3PO4 (37 mg, 0.262 mmol) and K2CO3 (90 mg, 0.655 mmol) were added and the reaction mixture was stirred for 18 h at 90° C. The reaction mixture was diluted with brine and extracted with EtOAc. The organic phase was dried with Na2SO4, filtered, concentrated under vacuum and purified by HPLC to give the title compound (7.6 mg). 1H-NMR (CDCl3, 400 MHz): δ: 7.91 (s, 1H), 7.71 (s, 1H), 7.50-7.60 (m, 3H), 7.12 (s, 1H), 7.08-7.10 (m, 2H), 7.01 (s, 1H), 4.57-4.61 (m, 1H), 3.79 (s, 3H), 3.46 (s, 3H), 1.82-1.98 (m, 1H), 1.78-1.82 (m, 1H), 0.82 (t, 3H, J=7.4 Hz); LCMS: 433.2 m/z (M+H)+; ret. Time: 4.36 min (Analytical Method C).

1. extractionextracted with EtOAc
2. dry with materialThe organic phase was dried with Na2SO4
3. filtrationfiltered
4. concentrationconcentrated under vacuum
5. custompurified by HPLC