HRID377135

反应详情

EQUATION

反应方程式

HRID 377135 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In 220 g of toluene, 20.3 g (0.883 mol) of sodium dispersion was reacted with 46.5 g (0.413 mol) of chlorobenzene, to prepare phenyl sodium. The resultant toluene slurry was stirred for 2.5 hours under heat reflux. The thus-obtained black slurry was cooled, and then a toluene (40 g) solution containing 31.6 g (0.413 mol) of allyl chloride was added to the cooled slurry, keeping the reaction temperature in the range of from -10° C. to 0° C., and then the reaction mixture was allowed to stand, for aging, for 30 minutes at room temperature. After the reaction was completed, the reaction mixture was subjected to hydrolysis with 350 ml of water in the range of 5 to 20° C., and then the resultant organic layer was washed with 300 ml of water twice, according to a usual manner. Toluene was removed therefrom by atomospheric distillation, and the residual orange oil was subjected to distillation under reduced pressure in the same manner as in Example 7. As a result, 39.4 g (0.298 mol, yield 72.2%) of 4-phenyl-1-butene was given (purity 98.3%), and 6.3 g of a residue remained.

WORKUP

后处理

  1. temperatureunder heat
  2. temperaturereflux
  3. temperatureThe thus-obtained black slurry was cooled
  4. additionwas added to the cooled slurry
  5. customof from -10° C. to 0° C.
  6. washthe resultant organic layer was washed with 300 ml of water twice
  7. customToluene was removed
  8. distillationby atomospheric distillation
  9. distillationthe residual orange oil was subjected to distillation under reduced pressure in the same manner as in Example 7