反応 #4244

反応方程式

4-allyl-2,6-dichlorophenyl glycidyl ether

peracetic acid

→

pale yellow resin

収率 92.3%

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

収率 92.3%

溶媒

toluene

sodium acetate

toluene

反応条件

後処理

1. 1
   その他equipped with stirrer
2. 2
   workup.ADDITIONAfter the dropwise addition
3. 3
   その他the resultant aqueous phase is separated
4. 4
   洗浄the organic phase is washed with two 150 ml portions of NaHCO3 (5%)
5. 5
   洗浄washed with 150 ml of water
6. 6
   乾燥The organic phase is dried over sodium sulfate
7. 7
   ろ過filtered
8. 8
   濃縮The filtrate is concentrated

実験手順

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.

出典