Reaktion #214223

Reaktionsgleichung

3-methyl-2-butenyl diazoacetate

→

(±)-6,6-dimethyl-2-oxo-3-oxabicyclo[3.1.0]hexane

Ausbeute 75.0%

Lösungsmittel

dioxane

dioxane

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONAfter completion of the addition
2. 2
   Temperaturthe reaction mixture was heated
3. 3
   Temperaturunder reflux for 1 hour
4. 4
   SonstigeThe crude reaction mixture
5. 5
   workup.DISTILLATIONwas distilled

Vorschrift

A solution of 3-methyl-2-butenyl diazoacetate (41.3 mmole, 6.36 g) in dioxane (20 ml) was added dropwise to a refluxing solution of cupric acetylacetonate (1.03 mmole, 0.27 g) in dioxane (400 ml) over a period of 7 hours under an argon atmosphere. After completion of the addition, the reaction mixture was heated under reflux for 1 hour. The crude reaction mixture was distilled to afford (±)-6,6-dimethyl-2-oxo-3-oxabicyclo[3.1.0]hexane (3.85 g, 75% yield); bp 110°, 16 mm Hg.

Quelle