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Hydrogen Bromide → 4(4-Chloro-3,5-dimethyl-phenoxy)-2,6-dimethyl-phenol

HRID 1074517
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HRID 1074517 반응식
[Cl:1][C:2]1[C:18]([CH3:19])=[CH:17][C:5]([O:6][C:7]2[CH:12]=[C:11]([CH3:13])[C:10]([O:14]C)=[C:9]([CH3:16])[CH:8]=2)=[CH:4][C:3]=1[CH3:20].Br>C(O)(=O)C>[Cl:1][C:2]1[C:18]([CH3:19])=[CH:17][C:5]([O:6][C:7]2[CH:8]=[C:9]([CH3:16])[C:10]([OH:14])=[C:11]([CH3:13])[CH:12]=2)=[CH:4][C:3]=1[CH3:20]
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참가 물질

4

반응물 2

HCID 260Hydrogen BromideHCID 127678104(4-Chloro-3,5-dimethyl-phenoxy)-2,6-dimethylanisole

생성물 1

HCID 127678094(4-Chloro-3,5-dimethyl-phenoxy)-2,6-dimethyl-phenol수율 102.4%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

40 g of 4(4-chloro-3,5-dimethyl-phenoxy)-2,6-dimethyl-anisole were added to a solution of 125 ml of 48% hydrobromic acid and 300 ml of glacial acetic acid. The mixture was then refluxed for 2 hours at the reflux condenser. After concentration under reduced pressure, water was added to the residue and the mixture was extracted with methylene chloride. After the organic extract had been shaken several times with water, it was concentrated and the residue was distilled under greatly reduced pressure. 39 g of 4(4-chloro-3,5-dimethyl-phenoxy)-2,6-dimethyl-phenol were obtained, boiling point: 186°-190° C. under a pressure of 2-3 mm mercury.

후처리

  1. temperatureThe mixture was then refluxed for 2 hours at the reflux condenser
  2. concentrationAfter concentration under reduced pressure, water
  3. additionwas added to the residue
  4. extractionthe mixture was extracted with methylene chloride
  5. extractionAfter the organic extract
  6. concentrationwas concentrated
  7. distillationthe residue was distilled under greatly reduced pressure

출처 및 근거

ORD 기록
ord-2db8d020323d4d22bf392b7ce1c42915
출처 데이터셋
uspto-grants-1983_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04391995

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