p-Chlorothiophenol → 2-(4-Chlorophenylthio)-1-(4-methylphenyl)ethanone

HRID 2187634

반응식

HRID 2187634 반응식
[CH3:1][C:2]1[CH:11]=[CH:10][C:5]([C:6](=[O:9])[CH2:7]Br)=[CH:4][CH:3]=1.[Cl:12][C:13]1[CH:18]=[CH:17][C:16]([SH:19])=[CH:15][CH:14]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[Cl:12][C:13]1[CH:18]=[CH:17][C:16]([S:19][CH2:7][C:6]([C:5]2[CH:10]=[CH:11][C:2]([CH3:1])=[CH:3][CH:4]=2)=[O:9])=[CH:15][CH:14]=1

참가 물질

5

반응물 3

HCID 7815p-ChlorothiophenolHCID 11430Potassium CarbonateHCID 692722-Bromo-4'-methylacetophenone

생성물 1

HCID 27451012-(4-Chlorophenylthio)-1-(4-methylphenyl)ethanone수율 82.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
80 °C

실험 절차

A mixture of 10.0 g (47 mmol) 4-methylphenacyl bromide, 6.8 g (47 mmol) 4-chlorothiophenol, and 6.5 g (47 mmol) anhydrous potassium carbonate in 100 ml dry DMF was stirred for 3 h at 80° C. It was filtered and the filtrate was concentrated under reduced pressure. The concentrate was stirred in water, and the resulting solid was filtered off, washed with water, and recrystallized from ethanol to give 10.7 g (82%) of the crude title compound.

후처리

  1. filtrationIt was filtered
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. stirringThe concentrate was stirred in water
  4. filtrationthe resulting solid was filtered off
  5. washwashed with water
  6. customrecrystallized from ethanol

출처 및 근거

ORD 기록
ord-44f50bf5ebd84717b40adb93417d9ac3
출처 데이터셋
uspto-grants-2002_06
특허 번호
US06410562B1

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