HRID1650019

反应详情

EQUATION

反应方程式

HRID 1650019 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a 2 liter three-neck flask equipped with a reflux condenser and a stirrer was added 50 ml of tetrahydrofuran which was dried with metallic sodium and 28 g (1.15 mole) of metallic magnesium and it was maintained with starring at room temperature. Then, a solution of 183 g (1.02 mole) of 3-vinylbenzene bromide in 500 ml of dry tetrahydrofuran was added dropwise over 2 hours to the above contents. The reaction temperature was maintained at 80° C. After the dropping of the solution, the stirring was continued for further 1 hour at 80° C. The thus obtained Grignard reagent solution was added dropwise over 2 hours to the solution of 171 g (1.0 mole) of benzyl bromide and 5.5 g of NiCl2 (Ph2P(CH)3PPh2) in 500 ml of dry ether Stirring was continued for further 1 hour at 35° C. This reaction mixture was poured into iced water and an oily layer was separated. Ether and tetrahydrofuran were evaporated off under reduced pressure to obtain (3-vinylphenyl)phenylmethane of the formula (I) in a yield of 60%.

WORKUP

后处理

  1. customTo a 2 liter three-neck flask equipped with a reflux condenser and a stirrer
  2. temperaturewas maintained
  3. customwith starring at room temperature
  4. waitwas continued for further 1 hour at 35° C
  5. customan oily layer was separated
  6. customEther and tetrahydrofuran were evaporated off under reduced pressure