反应详情

温度

60 °C

TFA (0.417 mL, 5.41 mmol) was added to a solution of 2-((2-chloro-5-cyano-3-(2-methyl-1-oxo-2,8-diazaspiro[4.5]decan-8-yl)phenyl)amino)-4-(cyclopropyl(4-methoxybenzyl)amino)imidazo[2,1-f][1,2,4]triazine-7-carbonitrile (50 mg, 0.078 mmol) and anisole (0.034 mL, 0.314 mmol) in DCE (1 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. 10 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-(2-methyl-1-oxo-2,8-diazaspiro[4.5]decan-8-yl)phenyl)amino)-4-(cyclopropylamino)imidazo[2,1-f][1,2,4]triazine-7-carbonitrile (17.4 mg).

1. customThe solvent was removed in vacuo
2. customthe material azeotroped with toluene 3×
3. customto remove the excess TFA
4. addition10 ml of 2N NH3 in MeOH was added
5. customThe solvent was removed in vacuo
6. customthe material was purified by prep-HPLC