Water → HCID 13373120, compound

HRID 257323Notes

Reaction equation

HRID 257323 reaction equation
[Cl:1][C:2]1[C:3]([N:12]2[C:16]([N:17](C(C)=O)[C:18]([CH3:20])=[O:19])=[C:15]([C:24]#[N:25])[CH:14]=[N:13]2)=[N:4][CH:5]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:7]=1.O>C(O)C>[Cl:1][C:2]1[C:3]([N:12]2[C:16]([NH:17][C:18]([CH3:20])=[O:19])=[C:15]([C:24]#[N:25])[CH:14]=[N:13]2)=[N:4][CH:5]=[C:6]([C:8]([F:10])([F:11])[F:9])[CH:7]=1

Participants

4

Reactant 2

HCID 962WaterHCID 13373119HCID 13373119, compound

Product 1

HCID 13373120HCID 13373120, compoundYield 77.6%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A stirred mixture of 0.32 gram (8.6×10-4 mole) of 1-(3-chloro-5-trifluoromethylpyridin-2-yl)-4-cyano-5-bis- (methylcarbonyl)aminopyrazole, 10 mL of water, and 10 mL of ethanol was heated at reflux for four hours. The mixture was cooled, and most of the ethanol was removed by distillation under reduced pressure. The aqueous pot residue, which contained a solid, was diluted with water, and the mixture was filtered. The filter cake was dried to yield 0.22 gram of 1-(3-chloro-5-trifluoromethylpyridin-2-yl)-4-cyano-5-methylcarbonylaminopyrazole. The rmr spectrum was consistent with the proposed structure.

Workup

  1. temperaturewas heated
  2. temperatureat reflux for four hours
  3. temperatureThe mixture was cooled
  4. custommost of the ethanol was removed by distillation under reduced pressure
  5. additionwas diluted with water
  6. filtrationthe mixture was filtered
  7. customThe filter cake was dried

Sources & evidence

ORD record
ord-023a1728517243319c4a9d702a7a2df3
Source dataset
uspto-grants-1993_11
Patent number
US05262382

Reaction notes

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