Potassium Carbonate → HCID 22934008, compound

HRID 1269728Notes

Reaction equation

HRID 1269728 reaction equation
C(=O)([O-])[O-].[K+].[K+].FC(F)(F)[C:9]([N:11]([C:13]1[CH:14]=[C:15]2[C:19](=[CH:20][CH:21]=1)[NH:18][N:17]=[CH:16]2)C)=O>CO.O>[CH3:9][NH:11][C:13]1[CH:14]=[C:15]2[C:19](=[CH:20][CH:21]=1)[NH:18][N:17]=[CH:16]2

Participants

5

Reactant 2

HCID 11430Potassium CarbonateHCID 22933660HCID 22933660, compound

Product 1

HCID 22934008HCID 22934008, compoundYield 100.2%

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 962WaterSolvent

Procedure

Potassium carbonate (8.64 g, 62.5 mmol) was added to a solution of 2,2,2-trifluoro-N-(1H-indazol-5-yl)-N-methylacetamide (3.80 g, 15.6 mmol) in a mixture of methanol (95 ml) and water (16 ml) at room temperature, and the resulting mixture was refluxed for 1.5 hours. Then, the reaction solution was concentrated and the resulting residue was poured into water and extracted with ethyl acetate. The organic layer was washed with a saturated aqueous sodium chloride solution and then dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain N-methyl-1H-indazol-5-amine (2.30 g, 100%).

Workup

  1. temperaturethe resulting mixture was refluxed for 1.5 hours
  2. concentrationThen, the reaction solution was concentrated
  3. additionthe resulting residue was poured into water
  4. extractionextracted with ethyl acetate
  5. washThe organic layer was washed with a saturated aqueous sodium chloride solution
  6. dry with materialdried over anhydrous magnesium sulfate
  7. distillationThe solvent was distilled off under reduced pressure

Sources & evidence

ORD record
ord-ed12b0c7cfd9418a80cc9cf3b89c2ab9
Source dataset
uspto-grants-2007_04
Patent number
US07199147B2

Reaction notes

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