HRID2225315

反应详情

EQUATION

反应方程式

HRID 2225315 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. stirringThe reaction mixture was then stirred at a room temperature for 2 hours
  2. additionthe reaction mixture was poured into a mixture of ice-concentrated hydrochloric acid
  3. extractionwas extracted with chloroform
  4. washThe chloroform layer was washed with water
  5. customdried
  6. customchloroform was removed from the reaction mixture by distillation
  7. customThe residue thus obtained
  8. customwas crystallized
  9. additionby adding isopropyl ether
  10. customthe crystals formed
  11. filtrationwere collected by filtration
  12. customrecrystallized from ethanol