Reacción #340514

ord-5c45bd272cda49449898c9d34baf01d7

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Extracciónextracted with ethyl acetate
  2. 2
    SecadoThe organic layer was dried over anhydrous magnesium sulfate
  3. 3
    workup.DISTILLATIONthe solvent was distilled off under reduced pressure
  4. 4
    Otrothe obtained residue was purified by silica gel column chromatography (eluent hexane:ethyl acetate=5:1)

Procedimiento

To a mixed solution of 20 g of 2,4-dimethyl-5-mercaptoaniline and 150 ml of N,N-dimethylformamide, 41 g of 2,2,2-trifluoroethyl iodide and 24 g of potassium carbonate were added, and 4 g of Rongalit was further added, followed by stirring at room temperature for 24 hours. The reaction mixture was poured into water and extracted with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure, and the obtained residue was purified by silica gel column chromatography (eluent hexane:ethyl acetate=5:1) to obtain 29 g of 2,4-dimethyl-5-(2,2,2-trifluoroethylthio)aniline.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07872036B2uspto-grants-2011_01