HRID1450252

反应详情

EQUATION

反应方程式

HRID 1450252 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

15 g of aluminium chloride are added with caution, at 0° C., to 25 g of 1,3-dibromobenzene in 250 ml of carbon disulphide, and 22.86 g of 2-bromopropionyl bromide are then run in slowly. The mixture is maintained at reflux for 8 hours, then the carbon disulphide is evaporated off under vacuum and the reaction medium is poured onto crushed ice. The product is extracted twice with heptane, dried, evaporated to dryness and then purified on a column of silica, using a mixture of cyclohexane and ethyl acetate (10:1 v/v) as eluent, to give the expected product.

WORKUP

后处理

  1. temperatureThe mixture is maintained
  2. temperatureat reflux for 8 hours
  3. customthe carbon disulphide is evaporated off under vacuum
  4. additionthe reaction medium is poured
  5. customonto crushed ice
  6. extractionThe product is extracted twice with heptane
  7. customdried
  8. customevaporated to dryness
  9. custompurified on a column of silica
  10. additiona mixture of cyclohexane and ethyl acetate (10:1 v/v) as eluent