Potassium Hydroxide → HCID 178526870, compound

HRID 622291Notes

Reaction equation

HRID 622291 reaction equation
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[C:4]([Cl:9])[C:3]=1[N:10]1[C:14](Cl)=[C:13]([N+:16]([O-:18])=[O:17])[CH:12]=[N:11]1.[OH-:19].[K+]>CO>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[C:4]([Cl:9])[C:3]=1[N:10]1[C:14]([OH:19])=[C:13]([N+:16]([O-:18])=[O:17])[CH:12]=[N:11]1

Participants

4

Reactant 2

HCID 14797Potassium Hydroxide2×HCID 136896085-Chloro-4-nitro-1-(2,4,6-trichlorophenyl)-1H-pyrazole

Product 1

HCID 178526870HCID 178526870, compoundYield 49%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

3.3 g of 1-(2,4,6-trichlorophenyl)-4-nitro-5-chloropyrazole are suspended in 10 ml of methanol, and 20 ml of 1N methanolic potassium hydroxide solution are added. The mixture is refluxed for 12 hours. In order to achieve complete reaction, a further 10 ml of 1N methanolic potassium hydroxide solution are added to the reaction mixture, which is refluxed for a further 12 hours. For work-up, the mixture is filtered, the solvent is stripped off in vacuo, the residue is taken up in hot water, and the product is precipitated by acidification with 2N hydrochloric acid. After filtering off and drying, 1.5 g (49% of theory) of 1-(2,4,6-trichlorophenyl)-4-nitro-5-hydroxypyrazole of melting point 106°-115° C. are obtained.

Workup

  1. temperatureThe mixture is refluxed for 12 hours
  2. customreaction
  3. temperatureis refluxed for a further 12 hours
  4. filtrationFor work-up, the mixture is filtered
  5. customthe product is precipitated by acidification with 2N hydrochloric acid
  6. filtrationAfter filtering off
  7. customdrying

Sources & evidence

ORD record
ord-82ca9ed688b44acfb09b731e9d104103
Source dataset
uspto-grants-1988_09
Patent number
US04770692

Reaction notes

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