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

HRID 846613

반응식

HRID 846613 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6d7d148d343648b0a8fd0c8b95b45100
출처 데이터셋
uspto-grants-1992_08
특허 번호
US05137897

연결된 노트

불러오는 중…