[5-(3-chloro-benzylamino)-2-methyl-2H-pyrazol-3-yl]-methanol → 5-(3-chloro-benzylamino)-2-methyl-2H-pyrazole-3-carbaldehyde

HRID 1367434노트

반응식

HRID 1367434 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:15]=[CH:16][CH:17]=1)[CH2:5][NH:6][C:7]1[CH:8]=[C:9]([CH2:13][OH:14])[N:10]([CH3:12])[N:11]=1>[O-2].[Mn+4].[O-2].ClCCl>[Cl:1][C:2]1[CH:3]=[C:4]([CH:15]=[CH:16][CH:17]=1)[CH2:5][NH:6][C:7]1[CH:8]=[C:9]([CH:13]=[O:14])[N:10]([CH3:12])[N:11]=1

참가 물질

4

반응물 1

HCID 57619232[5-(3-chloro-benzylamino)-2-methyl-2H-pyrazol-3-yl]-methanol

생성물 1

HCID 576191725-(3-chloro-benzylamino)-2-methyl-2H-pyrazole-3-carbaldehyde수율 60%

시약·촉매·용매 2

HCID 178418406HCID 178418406, 화합물촉매HCID 6344Dichloromethane용매

실험 절차

[5-(3-Chloro-benzylamino)-2-methyl-2H-pyrazol-3-yl]-methanol (647, 0.821 g, 3.26 mmol) was combined with dichloromethane (70 mL) and manganese(IV) oxide (4 g). The reaction was stirred at room temperature overnight under an atmosphere of nitrogen. The mixture was filtered through Celite and concentrated. Purification by silica gel column chromatography eluting with a gradient of ethyl acetate (10-100%) in hexane gave the desired aldehyde (648, 0.482 g, 60%).

후처리

  1. filtrationThe mixture was filtered through Celite
  2. concentrationconcentrated
  3. customPurification by silica gel column chromatography
  4. washeluting with a gradient of ethyl acetate (10-100%) in hexane

출처 및 근거

ORD 기록
ord-309e7bc01dd44bb98978e272f402c00e
출처 데이터셋
uspto-grants-2011_02
특허 번호
US07893075B2

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