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

HRID 1367434ノート

反応式

HRID 1367434 の反応式
[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

参加物

4

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 178418406HCID 178418406、化合物触媒HCID 6344Dichloromethane溶媒

実験手順

[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%).

後処理

  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

出典と根拠

ORDレコード
ord-309e7bc01dd44bb98978e272f402c00e
出典データセット
uspto-grants-2011_02
特許番号
US07893075B2

反応ノート

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