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Hydrochloric Acid → 1-(4-Bromo-3-fluorophenyl)cyclopropane-1-carboxylic acid

HRID 910880
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HRID 910880 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2([C:11]#N)[CH2:10][CH2:9]2)=[CH:4][C:3]=1[F:13].[OH-:14].[Na+].[OH:16]O.Cl>CO>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2([C:11]([OH:16])=[O:14])[CH2:10][CH2:9]2)=[CH:4][C:3]=1[F:13]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 784Hydrogen PeroxideHCID 14798Sodium HydroxideHCID 117156671-(4-Bromo-3-fluorophenyl)cyclopropane-1-carbonitrile

생성물 1

HCID 116518041-(4-Bromo-3-fluorophenyl)cyclopropane-1-carboxylic acid

시약·촉매·용매 1

HCID 887Methanol용매
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실험 절차

A suspension of 4-bromo-3-fluorophenylcyclopropanenitrile (21 mmoles) in methanol (10 ml) is added with a 35% NaOH aqueous solution (40 ml) and a 35% H2O2 aqueous solution (3 ml), then is refluxed for 4 hours, cooled at room temperature and added with 2N HCl (250 ml). The precipitated solid is collected by filtration and redissolved in a 5% NaHCO3 aqueous solution (300 ml). The insoluble fraction is filtered off and the clear filtrate is acidified to pH=2 with 2N HCl. The product precipitates as a white solid, which is recovered by filtration and dried under vacuum.

후처리

  1. filtrationThe precipitated solid is collected by filtration
  2. dissolutionredissolved in a 5% NaHCO3 aqueous solution (300 ml)
  3. filtrationThe insoluble fraction is filtered off
  4. customThe product precipitates as a white solid, which
  5. filtrationis recovered by filtration
  6. customdried under vacuum

출처 및 근거

ORD 기록
ord-36c41862430240dd916b45640b4899ad
출처 데이터셋
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08022250B2

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