Reaktion #165884

ord-627ac6ae4aef42b99e2567cbc7caaca5

Lösungsmittel

Reaktionsbedingungen

Temperatur
140°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas then heated
  2. 2
    TemperaturAfter cooling
  3. 3
    FiltrationThe precipitated crystal was collected by filtration
  4. 4
    Sonstigedried under reduced pressure at 60° C.

Vorschrift

In 250 mg of xylene were suspended 250 mg of phenyl 2-hydroxy-4,5-dimethoxybenzoate (3a) and 144 mg of methyl 2-amino-1,3-thiazole-4-carboxylate (4a) in a stream of argon, which was then heated to reflux (at 140° C.) for 7 hours. The reaction was not completed. After cooling, methanol was added, followed by stirring for one hour. The precipitated crystal was collected by filtration and dried under reduced pressure at 60° C. to provide 170 mg of the same compound (5a) as that of Example 4 at a yield of 55%.

Quelle

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