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Hydrochloric Acid → 4-methyl-5-phenyl-4H-1,2,4-triazole-3-thiol

HRID 257166
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HRID 257166 반응식
[C:1]([NH:9][NH:10][C:11]([NH:13][CH3:14])=[S:12])(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C([O-])(O)=O.[Na+].Cl>>[CH3:14][N:13]1[C:1]([C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)=[N:9][NH:10][C:11]1=[S:12]
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참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 27461131-Benzoyl-4-methyl-3-thiosemicarbazide

생성물 1

HCID 7197994-methyl-5-phenyl-4H-1,2,4-triazole-3-thiol

실험 절차

A stirred mixture of 1-benzoyl-4-methylthiosemicarbazide (20.9 g, 1.00×10-1 mole) and 1 molar aqueous NaHCO3 (1000 ml, 1 mole) was heated to reflux. After refluxing overnight the reaction was cooled in an ice bath. With stirring the solution was carefully acidified by the dropwise addition of conc. HCl (92 ml, 1.1 mole). A colorless precipitate formed and this was subsequently collected by filtration. Crystallization from ethanol afforded colorless, chunky crystals, Mp 164°-166° C.

후처리

  1. temperaturewas heated to reflux
  2. temperatureAfter refluxing overnight the reaction
  3. temperaturewas cooled in an ice bath
  4. customA colorless precipitate formed
  5. filtrationthis was subsequently collected by filtration
  6. customCrystallization from ethanol afforded colorless

출처 및 근거

ORD 기록
ord-92791f020f104e4283eafa221ee033dc
출처 데이터셋
uspto-grants-1993_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05260450

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