반응 #610411

ord-bb76bf10e5f3487caf2b26da65424186

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과The mixture was filtered
  2. 2
    농축the filtrate was concentrated
  3. 3
    세척washed with saturated aqueous NaHCO3
  4. 4
    기타The organic phase, with an insoluble precipitate, was separated from the aqueous phase
  5. 5
    농축concentrated

실험 절차

A mixture of N-(3-bromo-2-methylphenyl)-3,5-difluoro-2-nitrobenzamide (821 mg, 2.21 mmol), NH4Cl (1.18 g, 22.1 mmol) and zinc (1.45 g, 22.1 mmol) in MeOH (10 mL) was stirred at room temperature for 60 min. The mixture was filtered and the filtrate was concentrated. The residue was suspended in DCM and washed with saturated aqueous NaHCO3. The organic phase, with an insoluble precipitate, was separated from the aqueous phase and concentrated to give 2-amino-N-(3-bromo-2-methylphenyl) -3,5-difluorobenzamide (760 mg), used without further purification. Mass spectrum m/z 341, 343 (M+H)+, 363, 365 (M+Na)+.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09334290B2uspto-grants-2016_05