Reaktion #46492

ord-60a395f0ce344b469af603489c0c6e46

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    EinengenThe reaction solution was concentrated
  2. 2
    Extraktionextracted with EtOAc (2×100 mL)
  3. 3
    WaschenThe combined organic phases were washed with H2O
  4. 4
    Trocknendried over Na2SO4
  5. 5
    Einengenconcentrated
  6. 6
    SonstigePurification on silica gel

Vorschrift

A solution of the 2-amino-3-(bromomethyl)-5-bromopyridine hydrobromide salt (prepared above) in 40% aqueous methylamine (50 mL) and THF (50 mL) was stirred at RT overnight in a pressure bottle. The reaction solution was concentrated and extracted with EtOAc (2×100 mL). The combined organic phases were washed with H2O, dried over Na2SO4 and concentrated. Purification on silica gel afforded the title compound (4.25 g, 80%) as a yellow oil: MS (ES) m/e 217 (M+H)+.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07741339B2uspto-grants-2010_06