Réaction #74174

ord-fe6e1aa728a342208a1ca474b1c8918e

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Lavagewashed with water and brine
  2. 2
    Séchagedried over Na2SO4
  3. 3
    Autreevaporated to dryness
  4. 4
    AutreThe crude product was purified by chromatography on silica gel (n-hexane/ethyl acetate 7:3)

Mode opératoire

N-(3-acetyl-2,4-difluoro-phenyl)-2,5-difluoro-benzenesulfonamide (2.88 g, 8.293 mmol) was dissolved in dry DCM (75 mL) under nitrogen atmosphere. DIPEA (1.55 mL, 9.12 mmol, 1.1 eq) was then added, followed by 2-methoxyethoxymethyl chloride (0.98 mL, 9.12 mmol, 1.1 eq) and the mixture was stirred at room temperature for 1 h. It was then diluted with DCM and washed with water and brine, dried over Na2SO4 and evaporated to dryness. The crude product was purified by chromatography on silica gel (n-hexane/ethyl acetate 7:3) to give 2.25 g (62%) of N-(3-acetyl-2,4-difluoro-phenyl)-2,5-difluoro-N-(2-methoxy-ethoxymethyl)-benzene-sulfonamide as a yellow oil.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US08541575B2uspto-grants-2013_09