반응 #3778

반응 방정식

Amyl alcohol

2,3-dimethoxyphenol

2'-bromoacetophenone

potassium carbonate

→

2-(2,3-dimethoxyphenoxy)acetophenone

수율 87.0%

용매

ethyl acetate

반응 조건

후처리

1. 1
   온도by heating
2. 2
   세척the resulting solution was washed in dilute hydrochloric acid, in water
3. 3
   건조in a saturated sodium chloride solution, and dried over anhydrous magnesium sulfate
4. 4
   workup.DISTILLATIONthe solvents therein were distilled off under reduced pressure
5. 5
   기타The residue was purified by silica gel column chromatography (developing solvent: hexane:ethyl acetate=8:1)

실험 절차

Amyl alcohol (44 ml) was added to 2,3-dimethoxyphenol (5 g), 2'-bromoacetophenone (7 g), potassium carbonate (6.7 g) and copper acetate (1.1 g), followed by heating and stirring at 150° C. for 8 hours for reacting them together. To the reaction solution was added ethyl acetate (300 ml), and the resulting solution was washed in dilute hydrochloric acid, in water, and in a saturated sodium chloride solution, and dried over anhydrous magnesium sulfate, and the solvents therein were distilled off under reduced pressure. The residue was purified by silica gel column chromatography (developing solvent: hexane:ethyl acetate=8:1), to recover 2-(2,3-dimethoxyphenoxy)acetophenone (7.6 g; yield of 87%). By 1H-NMR (90 MHz, CDCl3), the compound has the peaks shown below.

출처