Reaktion #47748

ord-c39083f9bc564119906ee9e5f471c5d3

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe solution was filtered
  2. 2
    Sonstigeevaporated under vacuum
  3. 3
    SonstigeThe obtained residue was crystallized from ethanol

Vorschrift

4,5-Bis(bromomethyl)-3-hydroxy-2-methylpyridine (2)(3 g, 0.008 mol) was stirred in water (24 ml) at 45-50° C. for 40 min. The solution was filtered and evaporated under vacuum. The obtained residue was crystallized from ethanol. The yield was 1.2 g (50%). The position of bromomethyl- in pyridine-ring was verified by qualitative analysis with 2,6-dichloroquinone-4-chloroimide (Harris and Folkers (1939) J. Am. Chem. Soc. 61: 247). M.p. 158-159° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07745426B2uspto-grants-2010_06