Reaktion #2053488

Reaktionsgleichung

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

Lösungsmittel

THF

Reaktionsbedingungen

Aufarbeitung

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

Vorschrift

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.

Quelle