HRID468904

反应详情

EQUATION

反应方程式

HRID 468904 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of ethyl vinyl ether (4.5 mL, 47 mmol, 4.9 equiv.) and rhodium(II) acetate dimer (20.0 mg, 45.2 μmol, 4.8 mol %) in DCM (20 mL) at ambient temperature was treated with ethyl 2-diazoacetate (1.00 mL, 9.51 mmol) in 0.1 mL portions over 10 mins, allowing effervescence to subside between additions. The resulting green solution was stirred at ambient temperature for 2 h and concentrated in vacuo. The residue was dissolved in diethyl ether and washed with water, and with brine, dried over magnesium sulfate, filtered and concentrated in vacuo to afford crude ethyl 2-ethoxycyclopropanecarboxylate as a golden yellow oil (1.36 g, 90%) which was used without further purification.

WORKUP

后处理

  1. concentrationconcentrated in vacuo
  2. dissolutionThe residue was dissolved in diethyl ether
  3. washwashed with water
  4. dry with materialwith brine, dried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo