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Hydroxyamine hydrochloride → 3,5-Difluoro-4-((hydroxyimino)methyl)benzonitrile

HRID 929912
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HRID 929912 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH:7]=[C:8]([F:12])[C:9]=1[CH:10]=O)[C:5]#[N:6].Cl.[NH2:14][OH:15].C([O-])(=O)C.[K+]>CO>[F:1][C:2]1[CH:3]=[C:4]([CH:7]=[C:8]([F:12])[C:9]=1[CH:10]=[N:14][OH:15])[C:5]#[N:6]
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참가 물질

5

반응물 3

HCID 443297Hydroxyamine hydrochlorideHCID 517044Potassium AcetateHCID 162182563,5-Difluoro-4-formylbenzonitrile

생성물 1

HCID 900148513,5-Difluoro-4-((hydroxyimino)methyl)benzonitrile수율 23.3%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
60 °C

실험 절차

A mixture of 3,5-difluoro-4-formylbenzonitrile (500 mg, 3.0 mmol), hydroxylamine hydrochloride (207 mg, 3.0 mmol) and potassium acetate (586 mg, 6.0 mmol) in methanol (10 mL) was heated to 60° C. for 1 h then concentrated in vacuo and purified by column chromatography (eluent: DCM) to afford 3,5-difluoro-4-((hydroxyimino)methyl)benzonitrile (130 mg, 0.7 mmol) as a white solid.

후처리

  1. concentrationthen concentrated in vacuo
  2. custompurified by column chromatography (eluent: DCM)

출처 및 근거

ORD 기록
ord-d6c74245b79441fd9cbd77aeeca64ec0
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09296725B2

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