Potassium Carbonate → HCID 18506763, compound

HRID 610255Notes

Reaction equation

HRID 610255 reaction equation
F[C:2]1[C:30]([CH3:31])=[C:29]([F:32])[C:28]([F:33])=[CH:27][C:3]=1[C:4]([C:6](=[CH:12][NH:13][C:14]1[C:19]([F:20])=[CH:18][C:17]([F:21])=[C:16]([NH:22][C:23]([CH3:26])([CH3:25])[CH3:24])[N:15]=1)[C:7]([O:9][CH2:10][CH3:11])=[O:8])=[O:5].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[C:23]([NH:22][C:16]1[N:15]=[C:14]([N:13]2[C:2]3[C:3](=[CH:27][C:28]([F:33])=[C:29]([F:32])[C:30]=3[CH3:31])[C:4](=[O:5])[C:6]([C:7]([O:9][CH2:10][CH3:11])=[O:8])=[CH:12]2)[C:19]([F:20])=[CH:18][C:17]=1[F:21])([CH3:25])([CH3:26])[CH3:24]

Participants

4

Reactant 2

HCID 11430Potassium CarbonateHCID 178471972HCID 178471972, compound

Product 1

HCID 18506763HCID 18506763, compound

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Conditions

Temperature
100 °C

Procedure

To the solution of 4.6 g of the thus obtained ethyl 2-(2,4,5-trifluoro-3-methylbenzoyl)-3-[6-(t-butylamino)-3,5-difluoropyridin-2-yl]aminoacrylate in 10 ml dimethylformamide was added 1.35 g of potassium carbonate, and the mixture was stirred at 100° C. for 50 minutes. The reaction solution was extracted by adding water and acetic acid, and the organic layer was collected and dried over magnesium sulfate. The solvent was distilled off, and the residue was collected by filtration with ethanol and washed with diethylether to obtain 2.6 g of the title compound as a pale yellow powder.

Workup

  1. extractionThe reaction solution was extracted
  2. additionby adding water and acetic acid
  3. customthe organic layer was collected
  4. dry with materialdried over magnesium sulfate
  5. distillationThe solvent was distilled off
  6. filtrationthe residue was collected by filtration with ethanol
  7. washwashed with diethylether

Sources & evidence

ORD record
ord-d676d4aa802145f2aab25b9c83b88ebf
Source dataset
uspto-grants-1999_12
Patent number
US05998436

Reaction notes

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