Reaktion #518560

ord-037189ab6d104c389d654dbf9e844fd6

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe reaction mixture was then filtered through celite,
  2. 2
    Einengenconcentrated
  3. 3
    workup.DISSOLUTIONthe residue dissolved in 50 mL CH2Cl2
  4. 4
    WaschenThe organic solution was washed with 50 mL water
  5. 5
    Trocknendried over magnesium sulfate
  6. 6
    Filtrationfiltered
  7. 7
    Einengenconcentrated

Vorschrift

To a solution of (3,5-dinitrophenyl) (4-bromophenyl)amine (0.34 g, 1.0 mmol) in ethanol (10 mL) was added indium (2.0 g, 17 mmol) followed by saturated ammonium chloride solution (3 mL) and the mixture stirred 12 h. At this time, TLC showed the reaction complete. The reaction mixture was then filtered through celite, concentrated and the residue dissolved in 50 mL CH2Cl2. The organic solution was washed with 50 mL water followed by 50 mL brine, dried over magnesium sulfate, filtered and concentrated to give 0.26 g (93%) of a brown oil, Rf 0.1 (1:1 hexane:ethyl acetate), which was carried directly to the next step.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06656971B2uspto-grants-2003_12