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1-Chloro-4-(chloromethyl)benzene → 1,3-Bis(4-chlorophenyl)-2,2-dimethylpropan-1-one

HRID 1380920
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HRID 1380920 반응식
[CH:1]([C:4]([C:6]1[CH:11]=[CH:10][C:9]([Cl:12])=[CH:8][CH:7]=1)=[O:5])([CH3:3])[CH3:2].[OH-].[K+].[Cl:15][C:16]1[CH:23]=[CH:22][C:19]([CH2:20]Cl)=[CH:18][CH:17]=1>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.C1(C)C=CC=CC=1>[Cl:15][C:16]1[CH:23]=[CH:22][C:19]([CH2:20][C:1]([C:4]([C:6]2[CH:7]=[CH:8][C:9]([Cl:12])=[CH:10][CH:11]=2)=[O:5])([CH3:3])[CH3:2])=[CH:18][CH:17]=1
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참가 물질

6

반응물 3

HCID 77231-Chloro-4-(chloromethyl)benzeneHCID 14797Potassium HydroxideHCID 728651-(4-Chlorophenyl)-2-methylpropan-1-one

생성물 1

HCID 132174061,3-Bis(4-chlorophenyl)-2,2-dimethylpropan-1-one수율 60%

시약·촉매·용매 2

HCID 74236Tetrabutylammonium Bromide촉매
HCID 1140
Toluene
용매
2회

실험 절차

85 g (0.466 mol) of 4-chlorophenyl isopropyl ketone, 31.3 g (0.56 mol) of potassium hydroxide and 5 g of tetrabutylammonium bromide in 120 ml of toluene are heated to the reflux temperature, and a solution of 75 g (0.466 mol) of 4-chlorobenzyl chloride in 60 ml of toluene is added dropwise. The reaction mixture is subsequently stirred under reflux for 12 hours, cooled and washed with water and the organic phase is dried over sodium sulphate and concentrated in vacuo. 81.5 g (60% of theory) of 4-chlorophenyl 4-chlorophenyl-tert.-butyl ketone of refractive index nD20 1.5711 are obtained.

후처리

  1. temperatureunder reflux for 12 hours
  2. temperaturecooled
  3. washwashed with water
  4. dry with materialthe organic phase is dried over sodium sulphate
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-d860cf3ced7f43c4b635423a57a43aac
출처 데이터셋
uspto-grants-1986_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04584308

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