反应详情

温度

70 °C

In a 48 mL sealed pressure vessel, was added 4-(4-methylpiperazin-1-yl)benzenamine (0.851 g, 4.45 mmol), potassium carbonate (1.03 g, 7.42 mmol), N,N-dimethylformamide (10 mL) and 4-(2-chloropyridin-3-yl)-2-(methylsulfonyl)pyrimidine (Step 1, 1.0 g). the vessel was heated to 70° C. for 22 hours, cooled to room temperature, diluted with water, extracted into ethyl acetate, washed 1× with water and 1× with NaCl solution. The organics were dried over magnesium sulfate, filtered through fritted Buchner funnel, and concentrated. The crude was chromatographed on silica gel using 15-60% 90:10:1 (CH2Cl2:MeOH:NH4OH/CH2Cl2) as a gradient. Concentrated the product fractions to yield 4-(2-chloropyridin-3-yl)-N-(4-(4-methylpiperazin-1-yl)phenyl)pyrimidin-2-amine as a brown solid. MS (M+H)+=381. Calc'd 380.87 for C20H21ClN6.

1. customIn a 48 mL sealed pressure vessel
2. temperaturecooled to room temperature
3. extractionextracted into ethyl acetate
4. washwashed 1× with water and 1× with NaCl solution
5. dry with materialThe organics were dried over magnesium sulfate
6. filtrationfiltered through fritted Buchner funnel
7. concentrationconcentrated
8. customThe crude was chromatographed on silica gel using 15-60% 90:10:1 (CH2Cl2:MeOH:NH4OH/CH2Cl2) as a gradient
9. concentrationConcentrated the product fractions