Acetic Anhydride → HCID 10490701、化合物

HRID 1488495ノート

反応式

HRID 1488495 の反応式
C(O[C:5](=[O:7])[CH3:6])(=O)C.[N+:8]([C:11]1[CH:16]=[CH:15][C:14]([NH:17][N:18]2[CH:22]=[N:21][N:20]=[CH:19]2)=[CH:13][CH:12]=1)([O-:10])=[O:9]>N1C=CC=CC=1>[C:5]([N:17]([N:18]1[CH:22]=[N:21][N:20]=[CH:19]1)[C:14]1[CH:13]=[CH:12][C:11]([N+:8]([O-:10])=[O:9])=[CH:16][CH:15]=1)(=[O:7])[CH3:6]

参加物

4

反応物 2

HCID 7918Acetic AnhydrideHCID 108458884-Nitrophenyl(1,2,4-triazol-4-yl)amine

生成物 1

HCID 10490701HCID 10490701、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

2.8 Milliliters of acetic anhydride was added to 15 ml of a pyridine solution containing 0.62 g of 4-[(4-nitrophenyl)amino]-4H-1,2,4-triazole at room temperature and the mixture was stirred for about 2 hours. After completion of reaction, the solvent was removed by distillation under reduced pressure, and a proper amount of an aqueous sodium hydrogencarbonate solution was added to the residue obtained, which was then extracted several times each with ethyl acetate. The ethyl acetate layer was washed with water and dried over anhydrous magnesium sulfate, and the solvent was removed by distillation under reduced pressure. The residue was purified by silica gel column chromatography to give 0.52 g of 4-[N-acetyl-N-(4-nitrophenyl)amino]-4H-1,2,4-triazole from the chloroform/methanol (100/1) eluate.

後処理

  1. customAfter completion of reaction
  2. customthe solvent was removed by distillation under reduced pressure
  3. additiona proper amount of an aqueous sodium hydrogencarbonate solution was added to the residue
  4. customobtained
  5. extractionwhich was then extracted several times each with ethyl acetate
  6. washThe ethyl acetate layer was washed with water
  7. dry with materialdried over anhydrous magnesium sulfate
  8. customthe solvent was removed by distillation under reduced pressure
  9. customThe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-c598b818107a4bd88aa68bddeec8282c
出典データセット
uspto-grants-1997_10
特許番号
US05674886

反応ノート

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