反应详情

温度

125 °C

A mixture of 2,5-dimethyl-4-(1,4-dioxaspiro[4.5]decan-8-yl)aniline (111.3 mg, 0.43 mmol), 2-chloro-N-(5-methyl-1H-pyrazol-3-yl)-5-(trifluoromethyl)pyrimidin-4-amine (119.6 mg, 0.43 mmol), HCl (4 N in water, 0.11 mL, 0.43 mmol) in i-PrOH (4.0 mL) was heated at 125° C. in an oil bath over night. The reaction mixture was concentrated in vacuo. The crude product was dissolved in THF (2 mL), MeOH (1 mL) and HCl (4N in water, 0.11 mL, 0.43 mmol), and stirred at room temperature for 2 h. The reaction mixture was concentrated in vacuo, followed by purification by silica chromatography (0-100% EtOAc in hexanes gradient) to afford 4-(2,5-dimethyl-4-(4-(5-methyl-1H-pyrazol-3-ylamino)-5-(trifluoromethyl)pyrimidin-2-ylamino)phenyl)cyclohexanone; ESMS m/z 459.2 (M+H+).

1. concentrationThe reaction mixture was concentrated in vacuo
2. dissolutionThe crude product was dissolved in THF (2 mL)
3. concentrationThe reaction mixture was concentrated in vacuo
4. customfollowed by purification by silica chromatography (0-100% EtOAc in hexanes gradient)