HRID512582

反应详情

EQUATION

反应方程式

HRID 512582 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

Lead tetraacetate (5.7 g, 0.013 mol) and mercury (II) acetate (0.2 g, 0.0006 mol) are stirred together and thoroughly flushed with nitrogen. Chloroform (20 ml) is added and the dark orange solution heated to 50° C., followed by the addition of 4-benzyloxy-2,6-dimethylphenyl boronic acid (3 g, 0.012 mol) in one portion. After further heating at 50° C. for 3 hours the reaction mixture is cooled to 0° C. and potassium carbonate added (1.9 g, 0.02 mol). The suspension is stirred for just 5 minutes before filtering and evaporation of the crude solution under reduced pressure. The crude product is then azeotroped with diethyl ether to afford 4-benzyloxy-2,6-dimethylphenyl lead triacetate as a pale solid.

WORKUP

后处理

  1. customthoroughly flushed with nitrogen
  2. additionChloroform (20 ml) is added
  3. temperatureAfter further heating at 50° C. for 3 hours the reaction mixture
  4. temperatureis cooled to 0° C.
  5. filtrationbefore filtering
  6. customevaporation of the crude solution under reduced pressure
  7. customThe crude product is then azeotroped with diethyl ether