反应详情

To a solution of N4-[(trans-4-aminocyclohexyl)methyl]-N2-[2-(trifluoromethoxy)benzyl]-5-(trifluoromethyl)pyrimidine-2,4-diamine (100 mg, 0.22 mmol) in DMF (2 mL) were added 1,4-dibromobutane (140 mg, 0.65 mmol) and DIPEA (113 μL, 0.65 mmol). The reaction mixture was stirred at room temperature for 16 h and then heated at 65° C. for another 2 h. The reaction mixture was then diluted with EtOAc and washed with water (×4). The organic phase was dried over anhydrous Na2SO4 and concentrated in vacuo. The resulting residue was purified by silica gel preparative TLC using 10:1 CH2Cl2:MeOH as an eluent to afford 49 mg of the title compound as a while solid, m/z 518.6 [M+1]+.

1. temperatureheated at 65° C. for another 2 h
2. washwashed with water (×4)
3. dry with materialThe organic phase was dried over anhydrous Na2SO4
4. concentrationconcentrated in vacuo
5. customThe resulting residue was purified by silica gel preparative TLC