반응 #2053488

반응 방정식

diethyl azodicarboxylate

8-fluoro-3-iodocinnolin-4(1H)-one

3-methoxy-3-methylbutan-1-ol

triphenylphosphine

→

expected compound

8-Fluoro-3-iodo-1-(3-methoxy-3-methylbutyl)cinnolin-4(1H)-one

용매

THF

반응 조건

후처리

1. 1
   workup.WAITthe mixture is left
2. 2
   농축The reaction mixture is concentrated under vacuum
3. 3
   기타the residue is chromatographed on silica gel, elution

실험 절차

A mixture of 0.72 g of 8-fluoro-3-iodocinnolin-4(1H)-one and 0.48 ml of 3-methoxy-3-methylbutan-1-ol in 20 ml of THF is cooled to 5° C., 0.97 g of triphenylphosphine is added and then 0.65 g of diethyl azodicarboxylate is slowly added, and the mixture is left stirring overnight at AT. The reaction mixture is concentrated under vacuum and the residue is chromatographed on silica gel, elution being carried out with the cyclohexane/AcOEt mixture (75/25; v/v) and then with AcOEt. The expected compound is obtained.

출처