Water → 2-Bromo-1-[3,5-di(tert-butyl)-4-hydroxyphenyl]ethan-1-one

HRID 846613

反応式

HRID 846613 の反応式
[C:1]([C:5]1[CH:6]=[C:7]([C:16](=[O:18])[CH3:17])[CH:8]=[C:9]([C:12]([CH3:15])([CH3:14])[CH3:13])[C:10]=1[OH:11])([CH3:4])([CH3:3])[CH3:2].[Br:19]Br.O>C(Cl)Cl>[Br:19][CH2:17][C:16]([C:7]1[CH:6]=[C:5]([C:1]([CH3:4])([CH3:2])[CH3:3])[C:10]([OH:11])=[C:9]([C:12]([CH3:15])([CH3:14])[CH3:13])[CH:8]=1)=[O:18]

参加物

5

反応物 3

HCID 962WaterHCID 24408BromineHCID 6162963',5'-Bis(tert-butyl)-4'-hydroxyacetophenone

生成物 1

HCID 6161612-Bromo-1-[3,5-di(tert-butyl)-4-hydroxyphenyl]ethan-1-one

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

20.6 g (83 mmol) of 1-(3,5-di-tert.-butyl-4-hydroxy-phenyl)ethanone were dissolved in 50 ml of methylene chloride with stirring and heated to boiling, and 14.4 g (90 mmol) of bromine were added dropwise in the course of 15 minutes. The mixture was then heated under reflux for a further 2 hours and cooled, 50 ml of water were added, and the organic phase was separated and dried over sodium sulfate. After removing the solvent under reduced pressure, the solid residue was recrystallized from methylcyclohexane.

後処理

  1. temperatureheated
  2. temperatureThe mixture was then heated
  3. temperatureunder reflux for a further 2 hours
  4. temperaturecooled
  5. customthe organic phase was separated
  6. dry with materialdried over sodium sulfate
  7. customAfter removing the solvent under reduced pressure
  8. customthe solid residue was recrystallized from methylcyclohexane

出典と根拠

ORDレコード
ord-6d7d148d343648b0a8fd0c8b95b45100
出典データセット
uspto-grants-1992_08
特許番号
US05137897

関連ノート

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