반응 #4244

반응 방정식

4-allyl-2,6-dichlorophenyl glycidyl ether

peracetic acid

→

pale yellow resin

수율 92.3%

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

수율 92.3%

용매

toluene

sodium acetate

toluene

반응 조건

후처리

1. 1
   기타equipped with stirrer
2. 2
   workup.ADDITIONAfter the dropwise addition
3. 3
   기타the resultant aqueous phase is separated
4. 4
   세척the organic phase is washed with two 150 ml portions of NaHCO3 (5%)
5. 5
   세척washed with 150 ml of water
6. 6
   건조The organic phase is dried over sodium sulfate
7. 7
   여과filtered
8. 8
   농축The filtrate is concentrated

실험 절차

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.

출처