Methyl iodide → HCID 90384264, compound

HRID 928658Notes

Reaction equation

HRID 928658 reaction equation
C(=O)([O-])[O-].[K+].[K+].I[CH3:8].[Br:9][C:10]1[CH:15]=[C:14]([F:16])[C:13]([F:17])=[CH:12][C:11]=1[SH:18]>CN(C=O)C.C(OCC)(=O)C>[Br:9][C:10]1[CH:15]=[C:14]([F:16])[C:13]([F:17])=[CH:12][C:11]=1[S:18][CH3:8]

Participants

6

Reactant 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 50999469HCID 50999469, compound

Product 1

HCID 90384264HCID 90384264, compoundYield 95%

Reagents, catalysts & solvents 2

HCID 6228DimethylformamideSolventHCID 8857Ethyl AcetateSolvent

Procedure

Potassium carbonate (310 mg, 2.22 mmol) and iodomethane (0.138 mL, 2.22 mmol) were added to a solution (10 mL) of 2-bromo-4,5-difluorothiophenol (400 mg, 1.78 mmol) in DMF, and stirred at room temperature overnight. After diluted with ethyl acetate, the resultant was washed with water and saturated brine, and then dried over anhydrous magnesium sulfate. The solvent was distilled away, and the resulting residue was purified by silica gel chromatography (hexane/ethyl acetate) to thus obtain the title compound.

Workup

  1. washthe resultant was washed with water and saturated brine
  2. dry with materialdried over anhydrous magnesium sulfate
  3. distillationThe solvent was distilled away
  4. customthe resulting residue was purified by silica gel chromatography (hexane/ethyl acetate)

Sources & evidence

ORD record
ord-2b1eca77d06b4149b040defedaec879b
Source dataset
uspto-grants-2016_03
Patent number
US09290487B2

Reaction notes

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