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3-[3-Chloro-4-(hydroxymethyl)phenyl]-5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazole → 2-Chloro-4-[5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydro-isoxazol-3-yl]benzaldehyde

HRID 551314
ノート
印刷プレビュー

反応式

HRID 551314 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:10]2[CH2:14][C:13]([C:19]3[CH:24]=[C:23]([Cl:25])[CH:22]=[C:21]([Cl:26])[CH:20]=3)([C:15]([F:18])([F:17])[F:16])[O:12][N:11]=2)[CH:5]=[CH:6][C:7]=1[CH2:8][OH:9].[Cr](Cl)([O-])(=O)=O.[NH+]1C=CC=CC=1>ClCCl>[Cl:1][C:2]1[CH:3]=[C:4]([C:10]2[CH2:14][C:13]([C:19]3[CH:20]=[C:21]([Cl:26])[CH:22]=[C:23]([Cl:25])[CH:24]=3)([C:15]([F:18])([F:17])[F:16])[O:12][N:11]=2)[CH:5]=[CH:6][C:7]=1[CH:8]=[O:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 866315523-[3-Chloro-4-(hydroxymethyl)phenyl]-5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazoleHCID 178418287HCID 178418287、化合物

生成物 1

HCID 866315512-Chloro-4-[5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydro-isoxazol-3-yl]benzaldehyde収率 72.8%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

In a solution of 2.0 g of 3-[3-chloro-4-(hydroxymethyl)phenyl]-5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazole in 60 mL of dichloromethane, 4.0 g of silica gel and 1.3 g of pyridinium chlorochromate were added, and stirred at room temperature for 20 hours. After the completion of the reaction, the reaction mixture was filtered through glass filter in which silica gel was packed to separate a solid with a solvent. The solvent was distilled off under reduced pressure. The residual solid was washed with diisopropyl ether to obtain 1.45 g of the aimed product as pale yellow crystal.

後処理

  1. customAfter the completion of the reaction
  2. filtrationthe reaction mixture was filtered through glass
  3. filtrationfilter in which silica gel
  4. customto separate a solid with a solvent
  5. distillationThe solvent was distilled off under reduced pressure
  6. washThe residual solid was washed with diisopropyl ether

出典と根拠

ORDレコード
ord-772d74d16a814326992fb3b0243a9c4b
出典データセット
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07947715B2

反応ノート

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