反応 #3778

反応方程式

Amyl alcohol

2,3-dimethoxyphenol

2'-bromoacetophenone

potassium carbonate

→

2-(2,3-dimethoxyphenoxy)acetophenone

収率 87.0%

溶媒

ethyl acetate

反応条件

後処理

1. 1
   温度by heating
2. 2
   洗浄the resulting solution was washed in dilute hydrochloric acid, in water
3. 3
   乾燥in 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
   その他The residue was purified by silica gel column chromatography (developing solvent: hexane:ethyl acetate=8:1)

実験手順

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.

出典