反应详情

To a 0.30M solution of triphenylphosphine (1.5 eq) in THF was added di-tert-butylazodicarboxylate (1.5 eq). The mixture was stirred 15 min at ambient temperature. 4-Hydroxy-1-isopropylpiperidine (4.0 eq) was added. The mixture was stirred 15 min at ambient temperature. 2-Chloroquinazolin-8-ol (1.0 eq) was added. The mixture was stirred an additional 2 h. The crude mixture was concentrated, purified by flash chromatography (EtOAc then 90:10:1 DCM:MeOH:NH4OH), and concentrated to give the desired product in 88% yield. ES/MS m/z 306 (MH+).

1. stirringThe mixture was stirred 15 min at ambient temperature
2. stirringThe mixture was stirred an additional 2 h
3. concentrationThe crude mixture was concentrated
4. custompurified by flash chromatography (EtOAc
5. concentration90:10:1 DCM:MeOH:NH4OH), and concentrated