反应详情

温度

70 °C

tert-Butyl prop-2-ynylcarbamate (3.11 g), 4-chloro-5-iodo-6-methylpyrimidin-2-amine (1.8 g) and bis(triphenylphosphine)palladium(II) chloride (0.469 g) were combined in TEA (100 mL). The reaction mixture was purged with nitrogen gas for 3 min then copper(I) iodide (0.254 g) added. The resulting mixture was stirred at 70° C. for 16 h, then cooled to rt and filtered. The filtrate was washed with water and brine, dried and the solvents evaporated. The crude material was dissolved in MeOH (20 mL), acidified with acetic acid (1 mL) and purified by SCX and further purified by chromatography eluting 10% MeOH and 0.25% Ammonia (7N) in DCM to afford the subtitle compound 0.93 g.

1. customThe reaction mixture was purged with nitrogen gas for 3 min
2. additioncopper(I) iodide (0.254 g) added
3. temperaturecooled to rt
4. filtrationfiltered
5. washThe filtrate was washed with water and brine
6. customdried
7. customthe solvents evaporated
8. dissolutionThe crude material was dissolved in MeOH (20 mL)
9. custompurified by SCX
10. customfurther purified by chromatography
11. washeluting 10% MeOH and 0.25% Ammonia (7N) in DCM