Potassium Carbonate → HCID 18542928, compound

HRID 1276232Notes

Reaction equation

HRID 1276232 reaction equation
C(=O)([O-])[O-].[K+].[K+].[C:7]([C:9]1[CH:10]=[C:11]([NH:22][C:23](=[O:31])[C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=2[F:30])[CH:12]=[CH:13][C:14]=1[NH:15]C(=O)C(F)(F)F)#[N:8]>CO.O>[NH2:15][C:14]1[CH:13]=[CH:12][C:11]([NH:22][C:23](=[O:31])[C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=2[F:30])=[CH:10][C:9]=1[C:7]#[N:8]

Participants

5

Reactant 2

HCID 11430Potassium CarbonateHCID 18543575HCID 18543575, compound

Product 1

HCID 18542928HCID 18542928, compound

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 962WaterSolvent

Procedure

Potassium carbonate (5.0 g) is added to a solution of N-[3-cyano-4-(2,2,2-trifluoroacetyl-amino)-phenyl]-2-fluoro-benzamide (2.5 g) in methanol (270 mL) and water (16 mL) and the mixture is refluxed overnight. After removing the solvent under reduced pressure, the residue is suspended in water and extracted with dichloromethane. The organic extracts are pooled, washed with water and then saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure to provide the desired compound as a white solid.

Workup

  1. temperaturethe mixture is refluxed overnight
  2. customAfter removing the solvent under reduced pressure
  3. extractionextracted with dichloromethane
  4. washwashed with water
  5. dry with materialsaturated aqueous sodium chloride, dried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure

Sources & evidence

ORD record
ord-62cc5afadd0f4e9eb6e9b262806aabc7
Source dataset
uspto-grants-2000_12
Patent number
US06166028

Reaction notes

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