Reaktion #699554

ord-d6479b67cdfc4f32bef4a3c9d09a9e7d

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Waschenwashed successively with saturated potassium carbonate, saturated Na2S2O3 and brine
  2. 2
    Sonstigedried
  3. 3
    Einengenconcentrated
  4. 4
    WaschenFlash chromatography (eluting with hexane/ethyl acetate, 3:1 v/v) of the residual solid

Vorschrift

To a solution of 2-amino-5-chloropyridine (10 g) in acetic acid (75 mL) at r.t. was added bromine (2.6 mL) slowly. After 30 min, the acid was neutralized by the careful addition of sodium hydroxide (10 N) at 0° C. The resulting orange precipitate was dissolved in ethyl acetate and washed successively with saturated potassium carbonate, saturated Na2S2O3 and brine, dried and concentrated. Flash chromatography (eluting with hexane/ethyl acetate, 3:1 v/v) of the residual solid provided the title compound as a pale yellow solid (14.8 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06004950uspto-grants-1999_12