HRID847253

反应详情

EQUATION

反应方程式

HRID 847253 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

To a benzene solution (60 ml) of 4-(o-bromophenyl) butyric acid (5 g) was added oxalyl chloride (3.6 ml) and the reaction refluxed for 11/2 hrs. The solution was evaporated to dryness, the residue was dissolved in CH2Cl2 (50 ml) then cooled to 0° C., followed by the addition of AlCl3 (3.1 g). The mixture was stirred at 0° C. warming to room temperature overnight. The reaction was poured onto ice, then extracted with CH2Cl2. The organic layer was separated, washed with 1 N NaOH, then brine, separated, dried (MgSO4), filtered and evaporated affording the desired product (4.26 g).

WORKUP

后处理

  1. temperaturethe reaction refluxed for 11/2 hrs
  2. customThe solution was evaporated to dryness
  3. dissolutionthe residue was dissolved in CH2Cl2 (50 ml)
  4. additionfollowed by the addition of AlCl3 (3.1 g)
  5. temperaturewarming to room temperature overnight
  6. additionThe reaction was poured onto ice
  7. extractionextracted with CH2Cl2
  8. customThe organic layer was separated
  9. washwashed with 1 N NaOH
  10. custombrine, separated
  11. dry with materialdried (MgSO4)
  12. filtrationfiltered
  13. customevaporated