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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 542877
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HRID 542877 반응식
[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]
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참가 물질

3

반응물 1

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

생성물 1

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

시약·촉매·용매 1

HCID 260Hydrogen Bromide용매

실험 절차

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 pressure. 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.

후처리

  1. customthe mixture was evaporated to dryness under reduced pressure
  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

출처 및 근거

ORD 기록
ord-eb288b568d2e414b9efcf337b3879fca
출처 데이터셋
uspto-grants-1987_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04659729

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