HRID1722482

反应详情

EQUATION

反应方程式

HRID 1722482 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of the disodium salt of N-benzylazetidine-3,3-dicarboxylic acid and sodium carbonate (approximately 2:1 by weight, total weight 7.5 g) were dissolved in 100 ml of a toluene-acetic acid mixture (2/1, v/v), with immediate evolution of carbon dioxide from the sodium carbonate. The mixture was warmed and stirred, and then refluxed over a Dean and Stark water separator. After 1/2hour evolution of carbon dioxide had ceased and 1.5 ml of an acetic acid-water mixture had separated. The slightly hazy solution was cooled to room temperature. A white fluffy solid comprising sodium acetate (3.6 g) was removed by filtration. Distillation of the clear filtrate yielded 4.5 g of N-benzyl-3-carboxy-azetidine.

WORKUP

后处理

  1. temperatureThe mixture was warmed
  2. custom1.5 ml of an acetic acid-water mixture had separated
  3. customA white fluffy solid comprising sodium acetate (3.6 g) was removed by filtration
  4. distillationDistillation of the clear filtrate