HRID1781488

反应详情

EQUATION

反应方程式

HRID 1781488 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Glyoxylic acid (1.99 g, 27 mmol) and 1,3,5-triiso-propylbenzene (5.0 g, 24.5 mmol) were mixed in 30 mL glacial acetic acid and 2 mL concentrated sulfuric acid. The resulting solution was heated to reflux for 5 hours and then stirred at room temperature for 16 hours. The reaction mixture was poured into 100 g ice and the resulting mixture was extracted with diethyl ether. The organic layer was dried over MgSO4, filtered, and concentrated to give an oily solid which was recrystallized from hexanes to give 3.29 g of acetyloxy[2,4,6-tris(1-methylethyl)phenyl]acetic acid, mp 166°-169° C.

WORKUP

后处理

  1. temperatureThe resulting solution was heated
  2. temperatureto reflux for 5 hours
  3. extractionthe resulting mixture was extracted with diethyl ether
  4. dry with materialThe organic layer was dried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customto give an oily solid which
  8. customwas recrystallized from hexanes