1-Butanol → HCID 178491995, compound

HRID 2287084Notes

Reaction equation

HRID 2287084 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-9ab58afac5cb4d8e9df7d22d8871ef0b
Source dataset
uspto-grants-1981_05
Patent number
US04268680

Reaction notes

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