Reaktion #2386344

ord-7ca24c1c3bc84f3c8a8a0badc73d2607

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeReaction mixture
  2. 2
    Einengenwas concentrated in vacuo
  3. 3
    Sonstigeyielding an oil which
  4. 4
    Sonstigewas purified on silica gel column chromatography (CH2Cl2, neat)

Vorschrift

A solution of 2,4-dinitro-6-bromoaniline (1.6 g, 6.1 mmol), tetraethyltin (2.4 ml, 12.2 mmol) and Cl2Pd(PPh3)2 (100 mg) in 10 ml of DMF was stirred at 140° C. for 12 h. Reaction mixture was concentrated in vacuo, yielding an oil which was purified on silica gel column chromatography (CH2Cl2, neat) to provide 0.68 g (3.2 mmol, 53%) of 2,4-dinitro-6-ethylaniline, which was converted to the diamine (0.45 g, 95%) on hydrogenation (H2/Pd-C).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06495583B1uspto-grants-2002_12