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

HRID 1817669

반응식

HRID 1817669 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-cfb0ceb716d94b1f9d53368872319c4d
출처 데이터셋
uspto-grants-2009_10
특허 번호
US07598289B2

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