تفاعل #4244

ord-652355d8c729482398cb6fea03dd1456

معادلة التفاعل

C=CCc1cc(Cl)c(OCC2CO2)c(Cl)c1
4-allyl-2,6-dichlorophenyl glycidyl ether
CC(=O)OO
peracetic acid
Clc1cc(CC2CO2)cc(Cl)c1OCC1CO1
pale yellow resin
المردود 92.3%
Clc1cc(CC2CO2)cc(Cl)c1OCC1CO1
4-(2,3-Epoxypropyl)-2,6-dichlorophenyl glycidyl ether
المردود 92.3%

الكواشف

لا شيء

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىequipped with stirrer
  2. 2
    workup.ADDITIONAfter the dropwise addition
  3. 3
    أخرىthe resultant aqueous phase is separated
  4. 4
    غسيلthe organic phase is washed with two 150 ml portions of NaHCO3 (5%)
  5. 5
    غسيلwashed with 150 ml of water
  6. 6
    تجفيفThe organic phase is dried over sodium sulfate
  7. 7
    ترشيحfiltered
  8. 8
    تركيزThe filtrate is concentrated

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04724031uspto-grants-1988_02