反应详情

To a stirred solution of 1-[6-(2-amino-4-dimethylaminomethyl-phenylamino)-pyrimidin-4-yl]-3-(2,6-dichloro-3,5-dimethoxy-phenyl)-1-methyl-3-(2-trimethylsilanyl-ethoxymethyl)-urea in anhydrous DCM (10 mL) was added TFA (10 mL) at room temperature. The solution was stirred at room temperature for 3 hours. LCMS showed major product peak. The solution was evaporated to dryness, diluted with DCM (40 mL) and washed with 10% saturated Na2CO3 (10 mL). The DCM layer was dried over anhydrous Na2SO4. Concentration under vacuum gave crude product, which was purified by silica gel column chromatography (10% MeOH/DCM with 0.5% Et3N) to afford the title compound (45 mg, yield: 58% in two steps). MS (ESI): 520 [M+H]+.

1. customThe solution was evaporated to dryness
2. additiondiluted with DCM (40 mL)
3. washwashed with 10% saturated Na2CO3 (10 mL)
4. dry with materialThe DCM layer was dried over anhydrous Na2SO4
5. concentrationConcentration under vacuum
6. customgave crude product, which
7. customwas purified by silica gel column chromatography (10% MeOH/DCM with 0.5% Et3N)