Reaktion #165885

ord-b659c56f7db54725a1a56263bd05b943

Lösungsmittel

Reaktionsbedingungen

Temperatur
130°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONwas then added
  2. 2
    Temperaturby heating
  3. 3
    Temperaturto reflux for one hour
  4. 4
    SonstigeThe resultant reaction mixture
  5. 5
    Temperaturto cool
  6. 6
    Sonstigeby collecting the precipitated crystal
  7. 7
    Filtrationby filtration at 30° C.
  8. 8
    Sonstigelower before drying under reduced pressure

Vorschrift

In 1 mL of xylene were suspended 200 mg of 2-hydroxy-4,5-dimethoxybenzoic acid 4-nitrophenyl ester and 119 mg of 2-amino-1,3-thiazole-4-carboxylic acid methyl ester in a stream of argon, which was then stirred at 130° C. for 12 hours. The reaction mixture was allowed to stand to cool, to which 1 mL of methanol was then added, followed by heating to reflux for one hour. The resultant reaction mixture was allowed to stand to cool, followed by collecting the precipitated crystal by filtration at 30° C. or lower before drying under reduced pressure to provide 180 mg of the title compound (5a) at a yield of 80%.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08841461B2uspto-grants-2014_09