HRID649696

反应详情

EQUATION

反应方程式

HRID 649696 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Under a nitrogen atmosphere, 101.3 g (0.50 mole) of 3-chloro-2-methylbiphenyl (92% purity) in 75 g of dry tetrahydrofuran was added dropwise over two hours with stirring to a gently refluxing mixture of 13.1 g (0.54 mole) of fresh magnesium turnings, the heel from a previous run containing 0.21 mole of unreacted magnesium, and 75 g of dry tetrahydrofuran in a dry reaction vessel. Upon complete addition, the reaction mixture was heated at reflux for five additional hours. Gas chromatographic analysis of a quenched sample of the reaction mixture showed 1.2% of unreacted 3-chloro-2-methylbiphenyl and 92.4% of 2-methylbiphenyl. The reaction mixture was allowed to cool overnight.

WORKUP

后处理

  1. temperaturea gently refluxing
  2. customin a dry reaction vessel
  3. additionUpon complete addition
  4. temperaturethe reaction mixture was heated
  5. temperatureat reflux for five additional hours
  6. temperatureto cool overnight