HRID54709

反应详情

EQUATION

反应方程式

HRID 54709 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Trimethyl cyclopropane-1,2,3-tricarboxylate (20.6 g, 95.2 mmols) was dissolved in methanol (200 ml), followed by dropwise adding sodium hydroxide (23.7 g, 593 mmol) (dissolved in water (100 ml)) at room temperature, thereafter heating and reacting the mixture under reflux for one hour, cooling the reaction product, adding conc. hydrochloric acid (40 g, 1.1 mol), concentrating the reaction solution, adding acetone (200 ml) to the concentrated residue, heating the mixture under reflux for 2 hours, filtering off the precipitate, and concentrating the filtrate under reduced pressure, to obtain cyclopropane-1,2,3-tricarboxylic acid (16.0 g, 91.9 mmol, 97%).

WORKUP

后处理

  1. temperatureheating
  2. temperatureunder reflux for one hour
  3. temperaturecooling the reaction product
  4. concentrationconcentrating the reaction solution
  5. additionadding acetone (200 ml) to the concentrated residue
  6. temperatureheating the mixture
  7. temperatureunder reflux for 2 hours
  8. filtrationfiltering off the precipitate
  9. concentrationconcentrating the filtrate under reduced pressure