反応 #4243

反応方程式

4-allyl-2,6-dimethylphenyl glycidyl ether

formic acid

hydrogen peroxide

→

4-(2,3-epoxypropyl)-2,6-dimethylphenyl glycidyl ether

収率 85.5%

溶媒

chloroform

chloroform

反応条件

後処理

1. 1
   その他equipped with thermometer, stirrer, cooler and drip funnel
2. 2
   その他is held at this temperature overnight
3. 3
   洗浄the resultant solution is washed twice with 3% NaOH solution until neutral,
4. 4
   乾燥dried over sodium sulfate
5. 5
   ろ過filtered
6. 6
   濃縮The filtrate is concentrated

実験手順

A 350 ml sulfurating flask equipped with thermometer, stirrer, cooler and drip funnel is charged with 21.8 g (0.10 mole) of 4-allyl-2,6-dimethylphenyl glycidyl ether, 10.9 g (0.24 mole) of formic acid and 135 ml of chloroform. At room temperature, 23.2 g (0.47 mole) of hydrogen peroxide are then added dropise over 4 hours. The reaction miture is held at this temperature overnight. It is subsequently taken up in chloroform and the resultant solution is washed twice with 3% NaOH solution until neutral, made peroxide-free with sodium sulfite, dried over sodium sulfate and filtered. The filtrate is concentrated, affording 20.03 g (80.50% of theory) of 4-(2,3-epoxypropyl)-2,6-dimethylphenyl glycidyl ether in the form of a low viscous resin; epoxide content 7.7 equivalents/kg (90.11% of theory).

出典