Potassium Carbonate → HCID 178428726, compound

HRID 254823Notes

Reaction equation

HRID 254823 reaction equation
C(=O)([O-])[O-].[K+].[K+].Cl[C:8]1[CH:13]=[CH:12][C:11]([C:14]2[N:18]([C:19]3[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][C:20]=3[Cl:26])[N:17]=[C:16]([C:27]#[N:28])[C:15]=2[CH3:29])=[CH:10][CH:9]=1.[ClH:30].[NH2:31][OH:32]>CO>[Cl:30][C:8]1[CH:13]=[CH:12][C:11]([C:14]2[N:18]([C:19]3[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][C:20]=3[Cl:26])[N:17]=[C:16]([C:27](=[NH:28])[NH:31][OH:32])[C:15]=2[CH3:29])=[CH:10][CH:9]=1

Participants

5

Reactant 3

HCID 11430Potassium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 668444145-(4-chloro phenyl)-1-(2,4-dichlorophenyl)-4-methyl-1H-pyrazole-3-carbonitrile

Product 1

HCID 178428726HCID 178428726, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Conditions

Temperature
100 °C

Procedure

Potassium carbonate (0.58 g, 4.14 mmol) was added to a sealed tube containing a solution of 5-(4-chlorophenyl)-1-(2,4-dichlorophenyl)-4-methyl-1H-pyrazole-3-carbonitrile (1.0 g, 2.76 mmol) obtained in Step 2, hydroxylamine hydrochloride (0.39 g, 5.52 mmol) dissolved in MeOH (16 mL). The mixture was stirred vigorously and heated at 100° C. for 16 hr. The white precipitate formed was filtered and washed twice with cold water. It was further dried under a high vacuum. The filtrate was extracted with chloroform (30 mL×2), dried over MgSO4, filtered and evaporated under a vacuum, to obtain the title product in a compound amount of 1.04 g (2.63 mmol, 95%).

Workup

  1. customThe white precipitate formed
  2. filtrationwas filtered
  3. washwashed twice with cold water
  4. customIt was further dried under a high vacuum
  5. extractionThe filtrate was extracted with chloroform (30 mL×2)
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. customevaporated under a vacuum

Sources & evidence

ORD record
ord-f6e74b66d9cb43a8a67dce1d4658b289
Source dataset
uspto-grants-2011_01
Patent number
US07875647B2

Reaction notes

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