反应详情

温度

80 °C

To a stirred solution of 1,9-diazaspiro[5.5]undecan-2-one (TFA salt) (800 mg, 4.76 mmol) in 10 mL DMF, 2-chloroquinoxaline (937 mg, 5.71 mmol) and K2CO3 (3.3 g, 23.8 mmol) were added and the reaction mixture was stirred for 18 h at 80° C. under a nitrogen atmosphere. The reaction mixture was quenched with ice-cold water and extracted with ethyl acetate (2×50 mL), dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure. The crude mixture was purified by flash column chromatography (eluent: 3% methanol in chloroform) to yield the title compound (1.0 g, 71%). [LCMS RtF=0.37 min, [M+H]+=297.2]

1. customThe reaction mixture was quenched with ice-cold water
2. extractionextracted with ethyl acetate (2×50 mL)
3. dry with materialdried over anhydrous Na2SO4
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customThe crude mixture was purified by flash column chromatography (eluent: 3% methanol in chloroform)