反应详情

温度

60 °C

TFA (0.107 mL, 1.390 mmol) was added to a solution of 2-((2-chloro-5-cyano-3-(1,1-dioxidotetrahydro-2H-isothiazolo[2,3-a]pyrazin-5(3H)-yl)phenyl)amino)-4-(cyclopropyl(4-methoxybenzyl)amino)imidazo[2,1-f][1,2,4]triazine-7-carbonitrile (13 mg, 0.020 mmol) and anisole (8.80 μl, 0.081 mmol) in DCE (0.3 mL) and the reaction mixture was heated at 60° C. for 1 hours. The solvent was removed in vacuo and the material azeotroped with toluene 3× to remove the excess TFA. 2 ml of 2N NH3 in MeOH was added, and the solution was stirred for 20 min. The solvent was removed in vacuo and the material was purified by prep-HPLC to give 2-((2-chloro-5-cyano-3-(1,1-dioxidotetrahydro-2H-isothiazolo[2,3-a]pyrazin-5(3H)-yl)phenyl)amino)-4-(cyclopropylamino)imidazo[2,1-f][1,2,4]triazine-7-carbonitrile (5.1 mg)

1. customThe solvent was removed in vacuo
2. customthe material azeotroped with toluene 3×
3. customto remove the excess TFA
4. addition2 ml of 2N NH3 in MeOH was added
5. customThe solvent was removed in vacuo
6. customthe material was purified by prep-HPLC