反应详情

温度

140 °C

To the solution of (R)-8-cyclopentyl-7-ethyl-2-(2-fluoropyridin-4-yl)-5-methyl-7,8-dihydropteridin-6(5H)-one (Example 16, 200 mg, 0.56 mmol) in 5 mL of DMSO, (CH3)2NH HCl (200 mg 5.6 mmol) and Na2CO3 (130 mg, 1.2 mmol) were added. The mixture was heated to 140° C. for 18 hr in a sealed tube, quenched with water and extracted with EtOAc. The combined organic phase was dried with Na2SO4, concentrated under reduced pressure, and chromatographed (CH2Cl2:CH3OH=15:1) to give the title compound as a white solid (130 mg, 60% yield). 1H NMR (CDCl3) δ: 8.27 (d, 1H), 7.97 (s, 1H) 7.49 (s, 1H), 7.43 (d, 1H), 4.35-4.29 (m, 2H), 3.39 (s, 3H), 3.18 (s, 6H), 2.1-1.7 (m, 10H) and 0.87 ppm (t, 3H); LCMS: 381.3 m/z (M+H)+; ret. Time: 1.44 min (Analytical Method E).

1. customquenched with water
2. extractionextracted with EtOAc
3. dry with materialThe combined organic phase was dried with Na2SO4
4. concentrationconcentrated under reduced pressure
5. customchromatographed (CH2Cl2:CH3OH=15:1)