反应详情

温度

0 °C

To a solution of tert-butyl 4-(2-(ethylthio) quinazolin-7-yloxy)piperidine-1-carboxylate (1 eq) in THF (5 ml) was added a solution of oxone in water (5 ml) at 0° C. The reaction mixture was stirred for 30 min at 0° C. then warmed to room temperature and stirred for 4 h. The reaction was quenched with satd. sodium thiosulfate solution and basified with 1N NaOH. The product was extracted from basic layer with DCM. The DCM extracts were combined together, washed with brine and dried over sodium sulfate. The purification by flash column chromatography (70% EtOAc/Hexane) provide pure product in 60% yield. ES/MS m/z 422.0 (MH+).

1. temperaturethen warmed to room temperature
2. stirringstirred for 4 h
3. customThe reaction was quenched with satd
4. extractionThe product was extracted from basic layer with DCM
5. washwashed with brine
6. dry with materialdried over sodium sulfate
7. customThe purification by flash column chromatography (70% EtOAc/Hexane)
8. customprovide pure product in 60% yield