HRID132708

反应详情

EQUATION

反应方程式

HRID 132708 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 5.5 g pyrocatechol were added 50 ml tetrahydrofuran and 12.1 ml pyridine with stirring. Then to the resulting homogeneous mixture was slowly added 14.5 ml benzoyl chloride, and the reaction was stirred at room temperature for 1 hour, then heated refluxing for 4 hours. Next, 70 ml water was added to dissolve the resulting salt. The reaction mixture was extracted with toluene. Organic phase was separated, washed with saturated saline for two times, dried over anhydrous sodium sulfate. Removing solvent gave a white solid. After recrystallizing from ethyl acetate, 1,2-phenylene dibenzoate was obtained as a white crystal, the yield was 94%, and m.p. was 75-77° C.

WORKUP

后处理

  1. stirringthe reaction was stirred at room temperature for 1 hour
  2. temperatureheated
  3. temperaturerefluxing for 4 hours
  4. dissolutionto dissolve the resulting salt
  5. extractionThe reaction mixture was extracted with toluene
  6. customOrganic phase was separated
  7. washwashed with saturated saline for two times
  8. dry with materialdried over anhydrous sodium sulfate
  9. customRemoving solvent gave a white solid
  10. customAfter recrystallizing from ethyl acetate