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

HRID 1600574노트

반응식

HRID 1600574 반응식
[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

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 680234-FluorobenzaldehydeHCID 178418936HCID 178418936, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-c9fac0283cc24feab6f1a204ef003014
출처 데이터셋
uspto-grants-1999_11
특허 번호
US05977075

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