반응 #689419

반응 방정식

3-trifluoromethyl-5-trifluoromethanesulfonyl-1,2,-4-triazole

anisol

acetic anhydride

magnesium sulfate

→

p -methoxyacetophenone

수율 97.2%

용매

nitromethane

ether

반응 조건

후처리

1. 1
   여과After filtration on Celite
2. 2
   추출the solution was extracted with three fractions of 50 ml ether
3. 3
   세척the collected ether phase was washed with a saturated solution of potassium chloride
4. 4
   건조After drying the ether phase

실험 절차

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 .mu.moles) 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 NMR higher than 99%.

출처