1-Butanol → HCID 178491995, compound

HRID 971666Notes

Reaction equation

HRID 971666 reaction equation
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([NH:9][C:10]([NH:12][NH2:13])=[S:11])=[CH:5][CH:4]=1.Cl.[C:15](=N)(N)[CH3:16].C([O-])(=O)C.[Na+].C(O)CCC>O>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([N:9]2[C:15]([CH3:16])=[N:13][N:12]=[C:10]2[SH:11])=[CH:5][CH:4]=1

Participants

6

Reactant 4

HCID 2631-ButanolHCID 67170Acetamidine monohydrochlorideHCID 517045Sodium AcetateHCID 7371384-(4-Methoxyphenyl)-3-thiosemicarbazide

Product 1

HCID 178491995HCID 178491995, compoundYield 83%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

A mixture of 13.5 parts of N-(4-methoxyphenyl)hydrazinecarbothioamide, 15 parts of ethanimidamide hydrochloride, 15 parts of sodium acetate and 120 parts of 1-butanol is stirred and refluxed for 1 hour. The reaction mixture is cooled, 100 parts of water are added, followed by the addition of 140 parts of petroleumether. The precipitated product is filtered off and dried, yielding 12.5 parts (83%) of 4-(4-methoxyphenyl)-5-methyl-4H-1,2,4-triazole-3-thiol; mp. 214.2° C.

Workup

  1. temperaturerefluxed for 1 hour
  2. temperatureThe reaction mixture is cooled
  3. filtrationThe precipitated product is filtered off
  4. customdried

Sources & evidence

ORD record
ord-609c465b69b74b01bc2e6d768f4e1340
Source dataset
uspto-grants-1979_07
Patent number
US04160841

Reaction notes

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