Reaktion #165885
ord-b659c56f7db54725a1a56263bd05b943
Reaktionsgleichung
Edukte
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
130°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1workup.ADDITIONwas then added
- 2Temperaturby heating
- 3Temperaturto reflux for one hour
- 4SonstigeThe resultant reaction mixture
- 5Temperaturto cool
- 6Sonstigeby collecting the precipitated crystal
- 7Filtrationby filtration at 30° C.
- 8Sonstigelower 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%.