HRID2101516

反应详情

EQUATION

反应方程式

HRID 2101516 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred ice-cooled solution of triphenylphosphine in 10 mL of CH2Cl2 was added dropwise a solution of bromine in 5 ml of CH2Cl2. After the reaction mixture was stirred at room temperature for 30 min and cooled at ice bath temperature, a solution of the above (3-chloro-5-iodo-phenyl)-methanol in 15 ml of CH2Cl2 was added dropwise. The reaction mixture was stirred 0° C. for another 1 h and concentrated. The residue was washed with hexane several times and the combined hexane layer was concentrated to give 1-bromomethyl-3-chloro-5-iodo-benzene (1.2 g, 97%).

WORKUP

后处理

  1. temperaturecooled at ice bath temperature
  2. stirringThe reaction mixture was stirred 0° C. for another 1 h
  3. concentrationconcentrated
  4. washThe residue was washed with hexane several times
  5. concentrationthe combined hexane layer was concentrated