Potassium Carbonate → 4-(1H-1,2,3-Triazol-1-yl)benzaldehyde

HRID 1941345ノート

反応式

HRID 1941345 の反応式
[NH:1]1[CH:5]=[CH:4][N:3]=[N:2]1.C(=O)([O-])[O-].[K+].[K+].F[C:13]1[CH:20]=[CH:19][C:16]([CH:17]=[O:18])=[CH:15][CH:14]=1>N1C=CC=CC=1>[N:1]1([C:13]2[CH:20]=[CH:19][C:16]([CH:17]=[O:18])=[CH:15][CH:14]=2)[CH:5]=[CH:4][N:3]=[N:2]1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 680234-FluorobenzaldehydeHCID 178418936HCID 178418936、化合物

生成物 1

HCID 108449434-(1H-1,2,3-Triazol-1-yl)benzaldehyde

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A mixture of 1,2,3-triazole (3.4 ml, 58.7 mmol), potassium carbonate (9.03 g, 65.4 mmol), and 4-fluorobenzaldehyde (6.3 ml, 58.7 mmol) in pyridine (30 ml) is heated under nitrogen atmosphere at reflux overnight. After pyridine is distilled, the mixture is diluted with methylene chloride, filtered and washed with chloroform. The combined filtrate is washed with water, dried over magnesium sulfate, and concentrated in vacuo. The crude material is purified by column chromatography on silica with hexane/ethyl acetate (5:1) to give 4-(1,2,3-triazol-1-yl)-benzaldehyde and with hexane/ethyl acetate (1:2) to give 4-(1,2,3-triazol-1-yl)-benzaldehyde.

後処理

  1. temperatureis heated under nitrogen atmosphere
  2. temperatureat reflux overnight
  3. distillationAfter pyridine is distilled
  4. additionthe mixture is diluted with methylene chloride
  5. filtrationfiltered
  6. washwashed with chloroform
  7. washThe combined filtrate is washed with water
  8. dry with materialdried over magnesium sulfate
  9. concentrationconcentrated in vacuo
  10. customThe crude material is purified by column chromatography on silica with hexane/ethyl acetate (5:1)

出典と根拠

ORDレコード
ord-0f1d01cdfcef45f8b18c38c57d1c2017
出典データセット
uspto-grants-1997_12
特許番号
US05703106

反応ノート

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