Potassium Acetate → HCID 53679061, compound

HRID 366321Notes

Reaction equation

HRID 366321 reaction equation
[C:1]([C:4]1[O:5][C:6]2[C:12]([N:13]3[C:18](=[O:19])[CH:17]=[C:16]([C:20]([F:23])([F:22])[F:21])[N:15]([CH3:24])[C:14]3=[O:25])=[C:11]([F:26])[CH:10]=[C:9]([Cl:27])[C:7]=2[CH:8]=1)(=O)[CH3:2].C([O-])(=O)C.[K+].Cl.[CH3:34][O:35][NH2:36]>CO>[Cl:27][C:9]1[C:7]2[CH:8]=[C:4]([C:1](=[N:36][O:35][CH3:34])[CH3:2])[O:5][C:6]=2[C:12]([N:13]2[C:18](=[O:19])[CH:17]=[C:16]([C:20]([F:23])([F:22])[F:21])[N:15]([CH3:24])[C:14]2=[O:25])=[C:11]([F:26])[CH:10]=1

Participants

5

Reactant 3

HCID 517044Potassium AcetateHCID 521874O-Methylhydroxylamine hydrochlorideHCID 15477224HCID 15477224, compound

Product 1

HCID 53679061HCID 53679061, compoundYield 64.6%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

20 ml of methanol was added to 0.4 g (1 mmol) of 3-(2-acetyl-4-chloro-6-fluorobenzofuran-7-yl) -1-methyl-6-trifluoromethyluracil, 0.4 g (4 mmol) of potassium acetate and 0.33 g (4 mmol) of methoxyamine hydrochloride, followed by stirring at room temperature for 12 hours. After completion of the reaction, the solvent was distilled off under reduced pressure. The obtained residue was purified directly by silica gel column chromatography to obtain 0.28 g (yield: 64.6%) of the desired product as white powder. Melting point: 176-178° C.

Workup

  1. customAfter completion of the reaction
  2. distillationthe solvent was distilled off under reduced pressure
  3. customThe obtained residue was purified directly by silica gel column chromatography

Sources & evidence

ORD record
ord-48695a53616e4648996b416b99881887
Source dataset
uspto-grants-2000_10
Patent number
US06130187

Reaction notes

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