Reaktion #811211

ord-c037b52d27e5491bb05c1a91062c4ed9

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe resulting precipitates
  2. 2
    Filtrationwere collected by filtration
  3. 3
    Waschenwashed with water
  4. 4
    Sonstigedried under reduced pressure

Vorschrift

To a solution of 5-bromo-4,6-dimethyl-3-nitro-2-pyridinylamine (Heitsch, H.; et al. Bioorg. Med. Chem. 1997, 5, 673., 2.0 g, 8.1 mmol) in trifluoroacetic acid/water (v/v, 2:1, 30 mL) was added sodium nitrite (1.1 g, 16 mmol) in small portions at room temperature, and then the reaction mixture was stirred overnight. The resulting precipitates were collected by filtration, washed with water, and dried under reduced pressure to give 2.2 g (quant.) of the title compound: 1H-NMR (CDCl3) δ 2.53 (3H, s), 2.38 (3H, s).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07141580B2uspto-grants-2006_11