Реакция #4244

Уравнение реакции

4-allyl-2,6-dichlorophenyl glycidyl ether

peracetic acid

→

pale yellow resin

Выход 92.3%

4-(2,3-Epoxypropyl)-2,6-dichlorophenyl glycidyl ether

Выход 92.3%

Растворители

toluene

sodium acetate

toluene

Условия реакции

Обработка

1. 1
   Другоеequipped with stirrer
2. 2
   workup.ADDITIONAfter the dropwise addition
3. 3
   Другоеthe resultant aqueous phase is separated
4. 4
   Промывкаthe organic phase is washed with two 150 ml portions of NaHCO3 (5%)
5. 5
   Промывкаwashed with 150 ml of water
6. 6
   СушкаThe organic phase is dried over sodium sulfate
7. 7
   Фильтрацияfiltered
8. 8
   КонцентрированиеThe filtrate is concentrated

Методика

A 100 ml sulfurating flask equipped with stirrer, cooler, thermometer and drip funnel is charged with 13.0 g (0.05 mole) of 4-allyl-2,6-dichlorophenyl glycidyl ether in 40 ml of toluene and 0.5 g of sodium acetate. Over 2 hours, 14.0 g (0.07 mole) of 10% peracetic acid are then added dropwise at 30°-50° C. After the dropwise addition, the reaction mixture is diluted with 300 ml of toluene, the resultant aqueous phase is separated and the organic phase is washed with two 150 ml portions of NaHCO3 (5%) and then washed with 150 ml of water. The organic phase is dried over sodium sulfate and made peroxide-free with sodium sulfite and filtered. The filtrate is concentrated, affording 12.7 g (92.3%) of a pale yellow resin with an epoxide content of 5.62 eq/kg (77.75%) and a viscosity of 280 mPas/25° C.

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