HRID1076313

反应详情

EQUATION

反应方程式

HRID 1076313 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Sodium hydride (25.20 g., 0.60 mole, oil dispersion) is suspended in glyme (800 ml.) and phenyl acetone (80.50 g., 0.60 mole) in glyme (100 ml.) is added dropwise with stirring. After complete addition the mixture is heated to reflux for one hour. The mixture is cooled to room temperature and a solution of crude m-chlorocinnamyl bromide (139 g., 0.6 mole) in glyme (100 ml.) is added dropwise. When addition is complete the mixture is refluxed for 24 hours then allowed to cool. After filtration of inorganic salts and removal of solvent from the filtrate, vacuum distillation provides 36.11 g., b.p. 158.5°-163°/0.1 mm.

WORKUP

后处理

  1. additionAfter complete addition the mixture
  2. temperatureis heated
  3. temperatureto reflux for one hour
  4. additionWhen addition
  5. temperatureis refluxed for 24 hours
  6. temperatureto cool
  7. filtrationAfter filtration of inorganic salts and removal of solvent
  8. distillationfrom the filtrate, vacuum distillation
  9. customprovides 36.11 g