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Hydrochloric Acid → 1-[2-(4-Fluorophenyl)pyridin-4-yl]ethanone

HRID 1026758
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인쇄 미리보기

반응식

HRID 1026758 반응식
[CH3:1][Mg]Br.[F:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]2[CH:16]=[C:15]([C:17]#N)[CH:14]=[CH:13][N:12]=2)=[CH:7][CH:6]=1.Cl.[OH-:20].[Na+]>C(OCC)C.C(OCC)(=O)C>[F:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]2[CH:16]=[C:15]([C:17](=[O:20])[CH3:1])[CH:14]=[CH:13][N:12]=2)=[CH:7][CH:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 463120752-(4-Fluorophenyl)isonicotinonitrileHCID 178418573HCID 178418573, 화합물

생성물 1

HCID 866904831-[2-(4-Fluorophenyl)pyridin-4-yl]ethanone

시약·촉매·용매 2

HCID 3283Diethyl Ether용매
HCID 8857
Ethyl Acetate
용매

실험 절차

Methylmagnesium bromide (1.85 g) was added to a suspension of 2-(4-fluorophenyl)pyridine-4-carbonitrile (1.0 g) in diethyl ether (10 mL), and the mixture was stirred at room temperature overnight. After adding ice and 2M hydrochloric acid and stirring, the resulting mixture was made basic with 2M aqueous sodium hydroxide solution. After exracting with ethyl acetate, the organic phase was separated out and the solvent was distilled off The resulting residue was purified by column chromatography (silica gel cartridge, hexane:ethyl acetate=98:2-80:20) to afford 1-[2-(4-fluorophenyl)pyridin-4-yl]ethanone (350 mg).

후처리

  1. stirringstirring
  2. customthe organic phase was separated out
  3. distillationthe solvent was distilled off The resulting residue
  4. customwas purified by column chromatography (silica gel cartridge, hexane:ethyl acetate=98:2-80:20)

출처 및 근거

ORD 기록
ord-15c8269532ba4678b81e80489a24a818
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08729271B2

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