反应详情

温度

80 °C

To a stirring mixture of 7,8-bis(4-chlorophenyl)-[1,2,4]triazolo[4,3-a]pyridin-3(2H)-one (50 mg, 0.14 mmol) and K2CO3 (40 mg, 0.28 mmol) in DMF (0.47 mL) at 20° C. was added 4-bromobutane (40 mg, 0.28 mmol). The resulting reaction mixture was heated at 80° C. for 30 min. Analysis by HPLC/MS indicated that starting material had been consumed. The reaction mixture was brought to room temperature, diluted with water, and extracted twice with diethyl ether. The combined organic extract was washed with saturated aqueous NaHCO3 solution, then brine, then dried (MgSO4), filtered, and concentrated under reduced pressure. The crude product was purified by reverse phase preparative HPLC (acetonitrile-water-TFA) to isolate the title compound (18 mg, 0.044 mmol) as a light yellow solid. MS: [M+H]+=412.

1. customThe resulting reaction mixture
2. customhad been consumed
3. customwas brought to room temperature
4. additiondiluted with water
5. extractionextracted twice with diethyl ether
6. extractionThe combined organic extract
7. washwas washed with saturated aqueous NaHCO3 solution
8. dry with materialbrine, then dried (MgSO4)
9. filtrationfiltered
10. concentrationconcentrated under reduced pressure
11. customThe crude product was purified by reverse phase preparative HPLC (acetonitrile-water-TFA)