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

HRID 1155365
ノート
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反応式

HRID 1155365 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

40 g of 4(4-chloro-3,5-dimethyl-phenoxy)-2,6-dimethylanisole 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.

後処理

  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

出典と根拠

ORDレコード
ord-e9825c94285e49f78f21624c76679394
出典データセット
uspto-grants-1981_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04301295

反応ノート

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