反应详情

温度

115 °C

A vial was charged with 2-chloro-N-(5-cyclopropyl-1H-pyrazol-3-yl)pyrimidin-4-amine (100 mg, 0.42 mmol), tert-butyl (2-(((6-fluoro-1-(tetrahydro-2H-pyran-2-yl)-1H-indazol-4-yl)methyl)amino)ethyl)(methyl)carbamate (207 mg, 0.51 mmol), DIPEA (0.22 mL, 1.27 mmol) and n-BuOH (0.9 mL), sealed and heated at 115° C. for 4 d. The reaction mixture was then cooled to RT and 4N HCl/dioxane (1.06 mL, 4.24 mmol) was added. The reaction mixture was stirred at RT for 16 h then concentrated nvacuo. The crude mixture was purified by preparative HPLC to afford 22.4 mg (13%) of N4-(5-cyclopropyl-1H-pyrazol-3-yl)-N2-((6-fluoro-1H-indazol-4-yl)methyl)-N2-(2-(methylamino)ethyl)pyrimidine-2,4-diamine (II-47).

1. customsealed
2. temperatureThe reaction mixture was then cooled to RT
3. concentrationthen concentrated nvacuo
4. customThe crude mixture was purified by preparative HPLC