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3-ethyl-5-(4-methoxyphenyl)-4-phenyl-4H-1,2,4-triazole → 4-(3-ethyl-4-phenyl-4H-1,2,4-triazol-5-yl)-phenol

HRID 1981174
ノート
印刷プレビュー

反応式

HRID 1981174 の反応式
[CH2:1]([C:3]1[N:7]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[C:6]([C:14]2[CH:19]=[CH:18][C:17]([O:20]C)=[CH:16][CH:15]=2)=[N:5][N:4]=1)[CH3:2]>Br>[CH2:1]([C:3]1[N:7]([C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=2)[C:6]([C:14]2[CH:15]=[CH:16][C:17]([OH:20])=[CH:18][CH:19]=2)=[N:5][N:4]=1)[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 130540223-ethyl-5-(4-methoxyphenyl)-4-phenyl-4H-1,2,4-triazole

生成物 1

HCID 1357361664-(3-ethyl-4-phenyl-4H-1,2,4-triazol-5-yl)-phenol収率 88.5%

試薬・触媒・溶媒 1

HCID 260Hydrogen Bromide溶媒

実験手順

A solution of 3.86 g of 3-ethyl-5-(4-methoxyphenyl)-4-phenyl-4H-1,2,4-triazole and 20 ml of a hydrobromic acid solution at 48% was refluxed with stirring for one hour and the mixture was evaporated to dryness under reduced pressuure. The residue was dissolved in 20 ml of hot water and ammonium hydroxide was added until the pH was alkaline. The mixture was stood overnight with stirring and was vacuum. The product was washed with water and dried at 90° C. under reduced pressure. The 3.65 g of product were crystallized from methanol and the mixture was iced and vacuum filtered. The crystals were washed by empasting with methanol and were dried at 90° C. under reduced pressure to obtain 3.245 g of 4-(3-ethyl-4-phenyl-4H-1,2,4-triazol-5-yl)-phenol melting at 275° C.

後処理

  1. customthe mixture was evaporated to dryness under reduced pressuure
  2. dissolutionThe residue was dissolved in 20 ml of hot water
  3. additionammonium hydroxide was added until the pH
  4. waitThe mixture was stood overnight
  5. stirringwith stirring
  6. washThe product was washed with water
  7. customdried at 90° C. under reduced pressure
  8. customThe 3.65 g of product were crystallized from methanol
  9. filtrationvacuum filtered
  10. washThe crystals were washed
  11. customwere dried at 90° C. under reduced pressure

出典と根拠

ORDレコード
ord-2962a2707aea4ca48be2dfcf6561c200
出典データセット
uspto-grants-1985_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04512997

反応ノート

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