Reaktion #345746

ord-842e2554ff6647cd8bdc6689c98c502f

Lösungsmittel

Reaktionsbedingungen

Temperatur
170°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethe water is largely evaporated off
  2. 2
    ExtraktionWhile still moist the residue is extracted in the hot state twice with ethyl acetate
  3. 3
    SonstigeThe combined extracts are purified with active charcoal
  4. 4
    Sonstigethe solvent is then evaporated off

Vorschrift

A mixture of 12 parts of potassium hydroxide (85%), 200 parts of water, 10.4 parts of 2-amino-3-bromo-5-chloropyridine and 0.5 part of copper powder is stirred under nitrogen in an autoclave for 10 hours at 170° C. The aqueous solution is afterwards neutralised with concentrated hydrochloric acid and the water is largely evaporated off. While still moist the residue is extracted in the hot state twice with ethyl acetate. The combined extracts are purified with active charcoal, and the solvent is then evaporated off to leave 5 parts (70% of theory) of 2-amino-3-hydroxy-5-chloropyridine, m.p. 196°-201° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04033975uspto-grants-1977_07