反应详情

1259h. Into a 8-dram vial, N-{2-[2-Hydroxy-5-(2-trimethylsilanyl-ethoxymethoxy)-pyrrolo[2,1-f][1,2,4]triazin-7-yl]-phenyl}-N-methyl-methanesulfonamide (9.0E1 mg, 0.19 mmol), N,N-Dimethylformamide (0.70 mL, 9.0 mmol) N,N-Diisopropylethylamine (0.101 mL, 0.581 mmol) and N-Phenylbis(trifluoromethanesulphonimide) (83.0 mg, 0.232 mmol) were added. The reaction mixture was stirred at room temperature for one hour. 2-[4-(4-Amino-3-methoxy-phenyl)-piperidin-1-yl]-acetamide (102 mg, 0.387 mmol) was added. The reaction was heated at 120° C. for 3 hours. The solvent was removed under vacuum. The reaction mixture was purified via ISCO column chromatography with DCM and NH3 in methanol as eluant (2 to 15% NH3 in methanol). The collected fractions afforded 2-(4-{4-[7-[2-(Methanesulfonyl-methyl-amino)-phenyl]-5-(2-trimethylsilanyl-ethoxymethoxy)-pyrrolo[2,1-f][1,2,4]triazin-2-ylamino]-3-methoxy-phenyl}-piperidin-1-yl)-acetamide as a red oil (89 mg, 65%)

1. custom1259h
2. temperatureThe reaction was heated at 120° C. for 3 hours
3. customThe solvent was removed under vacuum
4. customThe reaction mixture was purified via ISCO column chromatography with DCM and NH3 in methanol as eluant (2 to 15% NH3 in methanol)