反应详情

A solution of ethyl 2-(4-aminophenoxy)acetate (0.801 g) and N-(3-((2-chloro-5-fluoropyrimidin-4-yl)amino)phenyl)acrylamide (1.0 g) in 1-butanol (10 mL) was heated to 135° C. for 2 hr. The reaction was monitored on TLC using hexanes:ethyl acetate (3:7) as mobile phase. After completion of the reaction, butanol was removed under reduced pressure and water was added. The mixture was extracted with ethyl acetate and the organic layer was dried over sodium sulfate and solvent was removed under reduced pressure. Crude material was purified by Combiflash chromatography and eluted with 29% ethyl acetate in hexane to give 0.30 g of ethyl 2-(4-((4-((3-acrylamidophenyl)amino)-5-fluoropyrimidin-2-yl)amino)phenoxy)acetate.

1. customwas removed under reduced pressure and water
2. additionwas added
3. extractionThe mixture was extracted with ethyl acetate
4. dry with materialthe organic layer was dried over sodium sulfate and solvent
5. customwas removed under reduced pressure
6. customCrude material was purified by Combiflash chromatography
7. washeluted with 29% ethyl acetate in hexane