Reaktion #313039

ord-260660ffa8214e8d954092ffdb7895ca

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Einengenwas concentrated
  2. 2
    workup.DISSOLUTIONthe residue was dissolved in CHCl3
  3. 3
    FiltrationThe resulting suspension was filtered
  4. 4
    Einengenthe filtrate was concentrated to a dark oil
  5. 5
    SonstigePurification on silica gel (EtOAc)

Vorschrift

To a solution of 2-amino-3-(hydroxymethyl)pyridine (13.0 g, 116.0 mmole) in CH2Cl2 (300 mL) at RT was added NBS (22.71 g, 127.6 mmole). After stirring at RT for 45 min the reaction solution was concentrated and the residue was dissolved in CHCl3. The resulting suspension was filtered and the filtrate was concentrated to a dark oil. Purification on silica gel (EtOAc) afforded the title compound (78%, 18.36 g) as a tan solid: MS (ES) m/e 204 (M+H)+.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07557125B2uspto-grants-2009_07