HRID339475

反应详情

EQUATION

反应方程式

HRID 339475 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of lead (IV) acetate (4.0 g, 0.0089 mol) and mercury (II) acetate (139 mg, 0.45 mmol) in chloroform (12 ml) at 50° C. is added 5-bromo-2-cyclopropylphenyl boronic acid (2.0 g, 0.0083 mol), and the solution is heated at this temperature for 5 hours. After cooling to room temperature the suspension is further cooled to 0° C. and anhydrous potassium carbonate (1.8 g) is added with rapid stirring for 2 minutes. The reaction mixture is then filtered (washing with additional chloroform), and the filtrate is concentrated to half its original volume and the crude product is precipitated with hexanes. Further concentration then filtration affords 5-bromo-2-cyclopropylphenyl lead triacetate as a beige solid.

WORKUP

后处理

  1. temperaturethe solution is heated at this temperature for 5 hours
  2. temperatureis further cooled to 0° C.
  3. filtrationThe reaction mixture is then filtered
  4. wash(washing with additional chloroform)
  5. concentrationthe filtrate is concentrated to half its original volume
  6. customthe crude product is precipitated with hexanes
  7. concentrationFurther concentration
  8. filtrationfiltration