HRID370569

反应详情

EQUATION

反应方程式

HRID 370569 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

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 atomosphere. 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.

WORKUP

后处理

  1. additionAfter completion of the addition
  2. temperaturethe reaction mixture was heated
  3. temperatureunder reflux for 1 hour
  4. customThe crude reaction mixture
  5. distillationwas distilled