HRID1184979

反应详情

EQUATION

反应方程式

HRID 1184979 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
160 °C

PROCEDURE

实验过程

10 ml of 95% concentrated sulfuric acid was slowly added dropwise into 5 ml of water, and the mixture was cooled to room temperature, to obtain a sulfuric acid solution. The prepared sulfuric acid solution was added into a three-necked flask containing 0.22 g of diethyl 2,3-diisopropyl-2-cyanosuccinate, and the reaction mixture was stirred at an oil-bath temperature of 160° C. for 16 h. Upon the completion of the reaction, the reaction mixture was cooled to room temperature, diluted with 30 ml of water, and cooled to room temperature again. The reaction mixture was extracted with anhydrous diethyl ether, and the solvent was removed from the extract liquor, to afford a mixture of white solids and oily liquid. This mixture was dissolved in 10 ml of 10% aqueous KOH solution, and the resultant solution was stirred at 50° C. for 45 min. The reaction mixture was extracted with diethyl ether, and the organic phase was discarded. The aqueous phase was acidified with concentrated hydrochloric acid, whereby white precipitates formed. The precipitates were filtered and dried, to afford the product, 2,3-diisopropyl succinic acid (yield: 60%).

WORKUP

后处理

  1. customUpon the completion of the reaction
  2. temperaturethe reaction mixture was cooled to room temperature
  3. temperaturecooled to room temperature again
  4. extractionThe reaction mixture was extracted with anhydrous diethyl ether
  5. customthe solvent was removed from the extract liquor
  6. customto afford
  7. additiona mixture of white solids and oily liquid
  8. extractionThe reaction mixture was extracted with diethyl ether
  9. customwhite precipitates
  10. customformed
  11. filtrationThe precipitates were filtered
  12. customdried