Peracetic Acid → 4-(2,3-Epoxypropyl)-2,6-dimethylphenyl glycidyl ether

HRID 4146노트

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HRID 4146 반응식
[CH2:1]([O:5][C:6]1[C:11]([CH3:12])=[CH:10][C:9]([CH2:13][CH:14]=[CH2:15])=[CH:8][C:7]=1[CH3:16])[CH:2]1[O:4][CH2:3]1.C([O-])(=[O:19])C.[Na+].C(OO)(=O)C>C(Cl)(Cl)Cl>[CH2:1]([O:5][C:6]1[C:7]([CH3:16])=[CH:8][C:9]([CH2:13][CH:14]2[O:19][CH2:15]2)=[CH:10][C:11]=1[CH3:12])[CH:2]1[O:4][CH2:3]1

참가 물질

5

반응물 3

HCID 6585Peracetic AcidHCID 517045Sodium AcetateHCID 198362214-Allyl-2,6-dimethylphenyl glycidyl ether

생성물 1

HCID 201527044-(2,3-Epoxypropyl)-2,6-dimethylphenyl glycidyl ether수율 863.5%

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

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).

후처리

  1. customequipped with thermometer, stirrer, cooler and drip funnel
  2. temperaturethe batch is heated to 35°-40° C
  3. washthe resultant solution is washed with 3% NaOH until neutral,
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. concentrationThe filtrate is concentrated by rotary evaporation

출처 및 근거

ORD 기록
ord-d41592ac9b864e5fa8d5045e4e4bc7fb
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04724031

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