反应详情

To a solution of tert-butyl (3-((5-fluoro-2-((4-(2-methoxyethoxy)phenyl)amino)pyrimidin-4-yl)amino)phenyl)carbamate (550 mg, 1.17 mmol) in DCM (20 mL) was added TFA (2 mL). Stirred for 30 min at rt for 4 h; removed solvent via rotary evaporation and partitioned oil with cold (0° C.) saturated sodium bicarbonate (10 mL) and EtOAc (10 mL), agitated and separated layers. Organic phase was dried over sodium sulfate and the solvent was removed via rotary evaporation to give a dark oil. Flash chromatography using 20%-100% Heptane/EtOAc gradient using combiflash system gave 309 mg of a light pink solid. LC/MS (RT=2.78/(M+1)) 370.2.

1. customremoved solvent via rotary evaporation
2. custompartitioned oil with cold (0° C.) saturated sodium bicarbonate (10 mL) and EtOAc (10 mL)
3. stirringagitated
4. customseparated layers
5. dry with materialOrganic phase was dried over sodium sulfate
6. customthe solvent was removed via rotary evaporation
7. customto give a dark oil