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4-Fluoro-3-[(3-fluorophenyl)-hydroxymethyl)-5-methoxybenzonitrile → HCID 22260967, 화합물

HRID 503169
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인쇄 미리보기

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HRID 503169 반응식
[F:1][C:2]1[C:9]([O:10][CH3:11])=[CH:8][C:5]([C:6]#[N:7])=[CH:4][C:3]=1[CH:12]([C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([F:20])[CH:15]=1)[OH:13]>C1(C)C=CC=CC=1.[O-2].[O-2].[Mn+4]>[F:1][C:2]1[C:9]([O:10][CH3:11])=[CH:8][C:5]([C:6]#[N:7])=[CH:4][C:3]=1[C:12](=[O:13])[C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([F:20])[CH:15]=1
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참가 물질

4

반응물 1

HCID 222606574-Fluoro-3-[(3-fluorophenyl)-hydroxymethyl)-5-methoxybenzonitrile

생성물 1

HCID 22260967HCID 22260967, 화합물수율 9.2%

시약·촉매·용매 2

HCID 178418406HCID 178418406, 화합물촉매HCID 1140Toluene용매

반응 조건

온도
60 °C

실험 절차

To a solution of 7.0 g of 4-fluoro-3-[(3-fluorophenyl)-hydroxymethyl]-5-methoxybenzonitrile in 70 ml toluene was added 11.1 g of activated manganese dioxide at room temperature. After stirring at 60° C. for one day, the manganese dioxide was filtered off through Celite. The solvent was removed and the crude product was purified and separated by silica gel column chromatography (ethyl acetate:n-hexane=1:3), to give 640 mg of the title compound as colorless crystals.

후처리

  1. filtrationthe manganese dioxide was filtered off through Celite
  2. customThe solvent was removed
  3. customthe crude product was purified
  4. customseparated by silica gel column chromatography (ethyl acetate:n-hexane=1:3)

출처 및 근거

ORD 기록
ord-1cbd791e3eb6452594788b53b6c89a15
출처 데이터셋
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07776890B2

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