تفاعل #4242

ord-d41592ac9b864e5fa8d5045e4e4bc7fb

معادلة التفاعل

C=CCc1cc(C)c(OCC2CO2)c(C)c1
4-allyl-2,6-dimethylphenyl glycidyl ether
CC(=O)[O-].[Na+]
sodium acetate
CC(=O)OO
peracetic acid
Cc1cc(CC2CO2)cc(C)c1OCC1CO1
4-(2,3-epoxypropyl)-2,6-dimethylphenyl glycidyl ether

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىequipped with thermometer, stirrer, cooler and drip funnel
  2. 2
    درجة الحرارةthe batch is heated to 35°-40° C
  3. 3
    غسيلthe resultant solution is washed with 3% NaOH until neutral,
  4. 4
    تجفيفdried over sodium sulfate
  5. 5
    ترشيحfiltered
  6. 6
    تركيزThe filtrate is concentrated by rotary evaporation

الإجراء التجريبي

A 350 ml sulfurating flask equipped with thermometer, stirrer, cooler and drip funnel is charged with 46.30 g (0.21 mole) of 4-allyl-2,6-dimethylphenyl glycidyl ether, 1.93 g of sodium acetate and 160 ml of chloroform, and the batch is heated to 35°-40° C. At this temperature, 52.3 g (0.28 mole) of 40% peracetic acid are then added dropwise over about 1 hour. The reaction mixture is then held at this temperature for a further 4 hours until the educt is no longer discernible in the gas chromatograph. When the reaction is complete, the reaction mixture is diluted in chloroform and the resultant solution is washed with 3% NaOH until neutral, made peroxide-free with sodium sulfite, dried over sodium sulfate and filtered. The filtrate is concentrated by rotary evaporation, affording 47.6 g of 4-(2,3-epoxypropyl)-2,6-dimethylphenyl glycidyl ether in the form of a low viscous oil; epoxide content 8.1 equivalents/kg (95.13% of theory).

المصدر

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