Acetic Anhydride → HCID 10490701, 화합물

HRID 1488495노트

반응식

HRID 1488495 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

HCID 10490701HCID 10490701, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c598b818107a4bd88aa68bddeec8282c
출처 데이터셋
uspto-grants-1997_10
특허 번호
US05674886

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