N-bromobutanimide → 4-Bromo-4-(4-chlorophenyl)-3,3-dimethylbutan-2-one

HRID 2119061노트

반응식

HRID 2119061 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([CH3:14])([CH3:13])[C:10](=[O:12])[CH3:11])=[CH:4][CH:3]=1.[Br:15]N1C(=O)CCC1=O>ClC(Cl)(Cl)Cl.N(C(C)(C)C#N)=NC(C)(C)C#N>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH:8]([Br:15])[C:9]([CH3:14])([CH3:13])[C:10](=[O:12])[CH3:11])=[CH:6][CH:7]=1

참가 물질

5

반응물 2

HCID 67184N-bromobutanimideHCID 128706324-(4-Chlorophenyl)-3,3-dimethylbutan-2-one

생성물 1

HCID 132771714-Bromo-4-(4-chlorophenyl)-3,3-dimethylbutan-2-one수율 82%

시약·촉매·용매 2

HCID 6547Azobisisobutyronitrile촉매HCID 5943Carbon Tetrachloride용매

실험 절차

50 g (0.237 mol) of 1-(4-chlorophenyl)-2,2-dimethyl-3-butanone are dissolved in 500 ml of tetrachloromethane, and 44.5 g (0.25 mol) of N-bromosuccinimide and 0.5 g of azobisisobutyronitrile are added. The reaction mixture is heated to boiling under reflux until solid material no longer sinks to the bottom on switching off the stirrer. After cooling down, the succinimide is filtered off with suction, the solvent is distilled off from the filtrate under waterpump vacuum and the residue is distilled under high vacuum. 56.3 g (82% of theory) of 1-(4-chlorophenyl)-1-bromo-2,2-dimethyl-3-butanone of boiling point 112°-118° C./0.2 mbar are obtained.

후처리

  1. temperatureThe reaction mixture is heated
  2. temperatureunder reflux until solid material
  3. temperatureAfter cooling down
  4. filtrationthe succinimide is filtered off with suction
  5. distillationthe solvent is distilled off from the filtrate under waterpump vacuum
  6. distillationthe residue is distilled under high vacuum

출처 및 근거

ORD 기록
ord-41bd04e92b6d421d88bf0ff0df3a671d
출처 데이터셋
uspto-grants-1987_07
특허 번호
US04681952

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