Reaktion #4244

Reaktionsgleichung

4-allyl-2,6-dichlorophenyl glycidyl ether

peracetic acid

→

pale yellow resin

Ausbeute 92.3%

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

Ausbeute 92.3%

Lösungsmittel

toluene

sodium acetate

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeequipped with stirrer
2. 2
   workup.ADDITIONAfter the dropwise addition
3. 3
   Sonstigethe resultant aqueous phase is separated
4. 4
   Waschenthe organic phase is washed with two 150 ml portions of NaHCO3 (5%)
5. 5
   Waschenwashed with 150 ml of water
6. 6
   TrocknenThe organic phase is dried over sodium sulfate
7. 7
   Filtrationfiltered
8. 8
   EinengenThe filtrate is concentrated

Vorschrift

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.

Quelle