反应详情

温度

60 °C

To a solution of 1-(7,8-bis(4-chlorophenyl)-3-oxo-2,3-dihydro-[1,2,4]triazolo[4,3-c]pyrimidin-5-yl)-3-(ethylamino)azetidine-3-carboxamide (25 mg, 0.05 mmol) in DMF (0.5 mL) at room temperature under argon was added K2CO3 (10 mg, 0.07 mmol), followed by iodoethane (10 mg, 0.064 mmol). The reaction mixture was stirred at 60° C. in a pre-heated oil bath for 30 min. After the reaction mixture was cooled to room temperature, water (5 mL) and EtOAc (5 mL) were added. The layers were separated. The organic layer was dried (MgSO4), filtered, and concentrated under reduced pressure. The crude product thus obtained was purified by preparative reverse phase HPLC (without TFA) to obtain 21.5 mg of the title compound as a white solid. HPLC/MS: retention time=3.465 min, [M+H]30 =526.

1. temperatureAfter the reaction mixture was cooled to room temperature
2. customThe layers were separated
3. dry with materialThe organic layer was dried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customThe crude product thus obtained
7. customwas purified by preparative reverse phase HPLC (without TFA)