Hydrochloric Acid → 1-(4'-Fluoro(1,1'-biphenyl)-4-yl)ethanone

HRID 2101230

반응식

HRID 2101230 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[CH:4][CH:3]=1.[Al+3].[Cl-].[Cl-].[Cl-].[N+](C1C=CC=CC=1)([O-])=O.[C:27](Cl)(=[O:29])[CH3:28].Cl>O>[F:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH:13]=[CH:12][C:11]([C:27](=[O:29])[CH3:28])=[CH:10][CH:9]=2)=[CH:6][CH:7]=1

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 6367Acetyl chlorideHCID 7416NitrobenzeneHCID 94614-FluorobiphenylHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 6081141-(4'-Fluoro(1,1'-biphenyl)-4-yl)ethanone

시약·촉매·용매 1

HCID 962Water용매

실험 절차

4′-Fluoro-biphenyl (0.03 mol) was added to 1 M AlCl3 in nitrobenzene (40 mL, 0.04 mol) with chilling in an ice bath. Acetyl chloride (0.06 mol) was added dropwise and the mixture stirred overnight at room temperature. The dark solution was poured into a mixture of crushed ice (150 mL), water (25 mL) and HCl (50 mL). The aqueous phase was separated and the nitrobenzene removed by steam distillation to give a dark low melting solid. The solid was recrystallised from aqueous methanol to give the title compound. δC (CDCl3, 62.9 MHz): 26.7, 115.9 (d, J 21.5), 127.1, 129.0 (d, J=7.8), 135.8, 136.0 (d, J 2.9), 144.7, 163.0 (d, J 248.0) and 197.8.

후처리

  1. temperaturewith chilling in an ice bath
  2. customThe aqueous phase was separated
  3. customthe nitrobenzene removed by steam distillation
  4. customto give a dark low melting solid
  5. customThe solid was recrystallised from aqueous methanol

출처 및 근거

ORD 기록
ord-4e8acfa88412423aa97d6545f9d00741
출처 데이터셋
uspto-grants-2009_08
특허 번호
US07572825B2

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