HRID2308156

反应详情

EQUATION

反应方程式

HRID 2308156 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
21 °C

PROCEDURE

实验过程

The catalytic effect of the scandium salt of 3-trifluoromethyl-5-trifluoromethanesulfonyl-1,2,4-triazole, obtained in Example 3, relative to a reaction was evaluated in the following manner. In 40 ml of anhydrous nitromethane, there is added 592 mg (700 mmoles) of the scandium salt of 3-trifluoromethyl-5-trifluoromethanesulfonyl-1,2,4-triazole, and 1.08 g (10 mmoles) of anisol and 2.04 g of acetic anhydride. After stirring during 10 min at 21° C., the reaction mixture was diluted with 50 ml of ether and the reaction was inhibited by 100 ml of a saturated solution of sodium bicarbonate NaHCO3. After filtration on Celite, the solution was extracted with three fractions of 50 ml ether, and the collected ether phase was washed with a saturated solution of potassium chloride. After drying the ether phase with magnesium sulfate and evaporation, 1.46 g of p-methoxyacetophenone (97% yield) was collected, with a purity characterized by a proton RMN higher than 99%.

WORKUP

后处理

  1. filtrationAfter filtration on Celite
  2. extractionthe solution was extracted with three fractions of 50 ml ether
  3. washthe collected ether phase was washed with a saturated solution of potassium chloride
  4. dry with materialAfter drying the ether phase