反应详情

A solution of 4-(2-((tert-butyldimethylsilyl)oxy)ethoxy)aniline (4.02 g) and N-(3-((2-chloro-5-fluoropyrimidin-4-yl)amino)phenyl)acrylamide (4.0 g) in 1-butanol (10 mL) was heated to 135° C. for 3 hr. The reaction was monitored on TLC using CHCl3: methanol (9.5:0.5) 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. Organic layer was dried over sodium sulfate and solvent was removed under reduced pressure. Crude material was purified by Combiflash chromatography eluting with 2.5% methanol in CHCl3 to give 0.828 g of N-(3-((2-((4-(2-((tert-butyldimethylsilyl)oxy)ethoxy)phenyl)amino)-5-fluoropyrimidin-4-yl)amino)phenyl)acrylamide.

1. customwas removed under reduced pressure and water
2. additionwas added
3. extractionThe mixture was extracted with ethyl acetate
4. dry with materialOrganic layer was dried over sodium sulfate and solvent
5. customwas removed under reduced pressure
6. customCrude material was purified by Combiflash chromatography
7. washeluting with 2.5% methanol in CHCl3