Hydrochloric Acid → HCID 23720353, compound

HRID 1721055Notes

Reaction equation

HRID 1721055 reaction equation
[CH3:1][N:2]1[C:6]([C:7]([F:10])([F:9])[F:8])=[N:5][NH:4][C:3]1=S.OO.[S:14]([O-:17])([OH:16])=[O:15].[Na+:18].Cl>[OH-].[Na+]>[CH3:1][N:2]1[C:6]([C:7]([F:10])([F:9])[F:8])=[N:5][N:4]=[C:3]1[S:14]([O-:17])(=[O:16])=[O:15].[Na+:18]

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 784Hydrogen PeroxideHCID 12391662,4-Dihydro-4-methyl-5-(trifluoromethyl)-3H-1,2,4-triazole-3-thioneHCID 23665763Sodium Bisulfite

Product 1

HCID 23720353HCID 23720353, compoundYield 73%

Reagents, catalysts & solvents 1

HCID 14798Sodium HydroxideSolvent

Conditions

Temperature
40 °C

Procedure

25 g (0.14 mol) of 4-methyl-5-trifluoromethyl-2,4-dihydro-3H-1,2,4-triazole-3-thione are dissolved in 250 ml of 2.5-molar sodium hydroxide solution, and 46.5 g of a 35% strength hydrogen peroxide solution (0.48 mol of H2O2) are added in the course of 60 minutes at a reaction temperature of 40° C. to 45° C. (external cooling). The mixture is stirred for 6 hours at 40° C.; excess oxidant is then decomposed using sodium hydrogen sulphite, and the solution is acidified with 18-molar hydrochloric acid to a pH of 2. It is subsequently washed with ethyl acetate, and the aqueous solution is then concentrated under a water pump vacuum to approximately 200 ml. The solid obtained during cooling is isolated by filtration. 25 g (73% of theory) of sodium 4-methyl-5-trifluoromethyl-4H-1,2,4-triazole-3-sulphonate are obtained.

Workup

  1. washIt is subsequently washed with ethyl acetate
  2. concentrationthe aqueous solution is then concentrated under a water pump vacuum to approximately 200 ml
  3. customThe solid obtained
  4. temperatureduring cooling
  5. customis isolated by filtration

Sources & evidence

ORD record
ord-6ca1af6307f54d29afa62064fa289deb
Source dataset
uspto-grants-1996_04
Patent number
US05508420

Reaction notes

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