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

HRID 1488509
ノート
印刷プレビュー

反応式

HRID 1488509 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6252e39343ae4ecb8341066955ef80d5
出典データセット
uspto-grants-1997_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05674886

反応ノート

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