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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
A mixture of 50 g of methyl 3-phenylpropionate, 51.6 g of chloroacetyl chloride and 250 ml of dichloromethane was cooled to 0° C. The mixture was stirred at 0° to 10° C. and 122 g of aluminum chloride was added gradually into the mixture. The reaction mixture was then stirred at a room temperature for 2 hours. The reaction mixture was allowed to stand overnight, then the reaction mixture was poured into a mixture of ice-concentrated hydrochloric acid and was extracted with chloroform. The chloroform layer was washed with water, dried then chloroform was removed from the reaction mixture by distillation. The residue thus obtained was crystallized by adding isopropyl ether, and the crystals formed were collected by filtration, then recrystallized from ethanol to obtain 53.4 g of methyl 3-(4-chloroacetylphenyl)propionate in the form of needle-like crystals.
WORKUP
后处理
- stirringThe reaction mixture was then stirred at a room temperature for 2 hours
- additionthe reaction mixture was poured into a mixture of ice-concentrated hydrochloric acid
- extractionwas extracted with chloroform
- washThe chloroform layer was washed with water
- customdried
- customchloroform was removed from the reaction mixture by distillation
- customThe residue thus obtained
- customwas crystallized
- additionby adding isopropyl ether
- customthe crystals formed
- filtrationwere collected by filtration
- customrecrystallized from ethanol