HRID1076313
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionAfter complete addition the mixture
- temperatureis heated
- temperatureto reflux for one hour
- additionWhen addition
- temperatureis refluxed for 24 hours
- temperatureto cool
- filtrationAfter filtration of inorganic salts and removal of solvent
- distillationfrom the filtrate, vacuum distillation
- customprovides 36.11 g