HRID1781488
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe resulting solution was heated
- temperatureto reflux for 5 hours
- extractionthe resulting mixture was extracted with diethyl ether
- dry with materialThe organic layer was dried over MgSO4
- filtrationfiltered
- concentrationconcentrated
- customto give an oily solid which
- customwas recrystallized from hexanes