Реакция #4242

Уравнение реакции

4-allyl-2,6-dimethylphenyl glycidyl ether

sodium acetate

peracetic acid

→

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

Растворители

chloroform

chloroform

Условия реакции

Обработка

1. 1
   Другоеequipped with thermometer, stirrer, cooler and drip funnel
2. 2
   Температураthe batch is heated to 35°-40° C
3. 3
   Промывкаthe resultant solution is washed with 3% NaOH until neutral,
4. 4
   Сушкаdried over sodium sulfate
5. 5
   Фильтрацияfiltered
6. 6
   КонцентрированиеThe filtrate is concentrated by rotary evaporation

Методика

A 350 ml sulfurating flask equipped with thermometer, stirrer, cooler and drip funnel is charged with 46.30 g (0.21 mole) of 4-allyl-2,6-dimethylphenyl glycidyl ether, 1.93 g of sodium acetate and 160 ml of chloroform, and the batch is heated to 35°-40° C. At this temperature, 52.3 g (0.28 mole) of 40% peracetic acid are then added dropwise over about 1 hour. The reaction mixture is then held at this temperature for a further 4 hours until the educt is no longer discernible in the gas chromatograph. When the reaction is complete, the reaction mixture is diluted in chloroform and the resultant solution is washed with 3% NaOH until neutral, made peroxide-free with sodium sulfite, dried over sodium sulfate and filtered. The filtrate is concentrated by rotary evaporation, affording 47.6 g of 4-(2,3-epoxypropyl)-2,6-dimethylphenyl glycidyl ether in the form of a low viscous oil; epoxide content 8.1 equivalents/kg (95.13% of theory).

Источник