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[3-(methylamino)-1-phenyl-1H-pyrazol-4-yl]methanol → 3-(methylamino)-1-phenyl-1H-pyrazole-4-carbaldehyde

HRID 2221654
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HRID 2221654 반응식
[CH3:1][NH:2][C:3]1[C:7]([CH2:8][OH:9])=[CH:6][N:5]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[N:4]=1>[O-2].[O-2].[Mn+4].O1CCCC1>[CH3:1][NH:2][C:3]1[C:7]([CH:8]=[O:9])=[CH:6][N:5]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[N:4]=1
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참가 물질

4

반응물 1

HCID 69217492[3-(methylamino)-1-phenyl-1H-pyrazol-4-yl]methanol

생성물 1

HCID 230763643-(methylamino)-1-phenyl-1H-pyrazole-4-carbaldehyde

시약·촉매·용매 2

HCID 178418406HCID 178418406, 화합물촉매HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of [3-(methylamino)-1-phenyl-1H-pyrazol-4-yl]methanol (15.42 g), activated manganese dioxide (50 g) and tetrahydrofuran (150 mL) was stirred at room temperature for 16 hrs. The obtained mixture was filtered, and the filtrate was concentrated. The residue was subjected to silica gel column chromatography to give 3-(methylamino)-1-phenyl-1H-pyrazole-4-carbaldehyde as colorless crystals from a fraction eluted with ethyl acetate-hexane (1:4, v/v). Recrystallization from ethyl acetate-hexane gave colorless needle crystal (9.17 g, yield 60%). melting point: 83-84° C.

후처리

  1. filtrationThe obtained mixture was filtered
  2. concentrationthe filtrate was concentrated

출처 및 근거

ORD 기록
ord-d9459743dd9e4c50905fa4a369406992
출처 데이터셋
uspto-grants-2008_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07368578B2

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