Reaktion #446032

ord-cf512ed7d25e4c498ac10272e7521869

Lösungsmittel

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONThe reaction solution is then poured onto ice
  2. 2
    Sonstigethe phases are separated
  3. 3
    SonstigeAfter some time the above acid crystallises out and
  4. 4
    Filtrationis filtered off with suction
  5. 5
    Sonstigedried

Vorschrift

12 g of potassium tert.-butoxide are added to a solution of 14 g of 6-(thiophen-3-yl)-pyridine-2,3-dicarboxylic acid diethyl ester and 6 g of 2-amino-2,3-dimethyl- butyramide in 100 ml of dry toluene while stirring and the solution is heated at 80° C. for 5 hours. The reaction solution is then poured onto ice, the phases are separated and the aqueous phase is acidified with 10 ml of glacial acetic acid. After some time the above acid crystallises out and is filtered off with suction and dried. In this manner 13.5 g of 6-(thiophen-3-yl)-2-(5-isopropyl-5-methyl-4-oxo-imidazol-2-yl)-pyridine-3-carboxylic acid having a melting point of 253°-257° C. are obtained.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04997947uspto-grants-1991_03