Sodium Hydroxide → HCID 178524446, compound

HRID 648902Notes

Reaction equation

HRID 648902 reaction equation
[C:1]([C:6]1[CH:11]=[CH:10][C:9]([N:12]2[CH:16]=[N:15][N:14]=[C:13]2[SH:17])=[CH:8][CH:7]=1)([O:3]CC)=[O:2].[OH-].[Na+]>O>[C:1]([C:6]1[CH:7]=[CH:8][C:9]([N:12]2[CH:16]=[N:15][N:14]=[C:13]2[SH:17])=[CH:10][CH:11]=1)([OH:3])=[O:2]

Participants

4

Reactant 2

HCID 14798Sodium HydroxideHCID 178468982HCID 178468982, compound

Product 1

HCID 178524446HCID 178524446, compoundYield 82.4%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

To 8.2 g of 1-(4-carboethoxyphenyl)-2-mercapto-1,3,4-triazole was added 50 ml of an aqueous solution of 2 mol/liter of sodium hydroxide and the mixture was refluxed for 1 hour. Then, 100 ml of water was added to the reaction mixture and after filtering away insoluble matter, the pH of the filtrate was adjusted to about 1 by the addition of hydrochloric acid. Crystals thus formed were collected by filtration, dissolved in 500 ml of N,N-dimethylformamide and ethyl acetate and hexane were added to the solution, whereby 6.0 g of 1-(4-carboxyphenyl)-2-mercapto-1,3,4-triazole was obtained. The yield was 82.2% and the melting point was above 300° C.

Workup

  1. temperaturethe mixture was refluxed for 1 hour
  2. filtrationafter filtering away insoluble matter
  3. additionthe pH of the filtrate was adjusted to about 1 by the addition of hydrochloric acid
  4. customCrystals thus formed
  5. filtrationwere collected by filtration
  6. dissolutiondissolved in 500 ml of N,N-dimethylformamide
  7. additionethyl acetate and hexane were added to the solution

Sources & evidence

ORD record
ord-dd435c05fda54a638848924288d1210e
Source dataset
uspto-grants-1988_04
Patent number
US04737452

Reaction notes

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