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Acetic Anhydride → 4-[N-(4-acetylaminophenyl)-N-(4-bromobenzyl)amino]-4H-1,2,4-triazole

HRID 1488509
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HRID 1488509 반응식
C(O[C:5](=[O:7])[CH3:6])(=O)C.[NH2:8][C:9]1[CH:14]=[CH:13][C:12]([N:15]([N:24]2[CH:28]=[N:27][N:26]=[CH:25]2)[CH2:16][C:17]2[CH:22]=[CH:21][C:20]([Br:23])=[CH:19][CH:18]=2)=[CH:11][CH:10]=1>N1C=CC=CC=1>[C:5]([NH:8][C:9]1[CH:14]=[CH:13][C:12]([N:15]([N:24]2[CH:25]=[N:26][N:27]=[CH:28]2)[CH2:16][C:17]2[CH:18]=[CH:19][C:20]([Br:23])=[CH:21][CH:22]=2)=[CH:11][CH:10]=1)(=[O:7])[CH3:6]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 229058094-[N-(4-aminophenyl)-N-(4-bromobenzyl)amino]-4H-1,2,4-triazole

생성물 1

HCID 229057974-[N-(4-acetylaminophenyl)-N-(4-bromobenzyl)amino]-4H-1,2,4-triazole

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

0.28 Milliliter of acetic anhydride was added to ml of a pyridine solution containing 0.35 g of 4-[N-(4-aminophenyl)-N-(4-bromobenzyl)amino]-4H-1,2,4-triazole at room temperature and the mixture was stirred for about minutes. After reaction, the solvent was removed by distillation under reduced pressure, and a proper amount of an aqueous sodium hydrogen carbonate solution was added to the resulting residue, which was then extracted 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 chromatography to obtain 0.33 g of 4-[N-(4-acetylaminophenyl)-N-(4-bromobenzyl)amino]-4H-1,2,4-triazole from the chloroform/methanol (50/1) eluate.

후처리

  1. customAfter reaction
  2. customthe solvent was removed by distillation under reduced pressure
  3. additiona proper amount of an aqueous sodium hydrogen carbonate solution was added to the resulting residue, which
  4. extractionwas then extracted with ethyl acetate
  5. washThe ethyl acetate layer was washed with water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customthe solvent was removed by distillation under reduced pressure
  8. customThe residue was purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-6252e39343ae4ecb8341066955ef80d5
출처 데이터셋
uspto-grants-1997_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05674886

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