反応 #165885

ord-b659c56f7db54725a1a56263bd05b943

溶媒

反応条件

温度
130°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONwas then added
  2. 2
    温度by heating
  3. 3
    温度to reflux for one hour
  4. 4
    その他The resultant reaction mixture
  5. 5
    温度to cool
  6. 6
    その他by collecting the precipitated crystal
  7. 7
    ろ過by filtration at 30° C.
  8. 8
    その他lower before drying under reduced pressure

実験手順

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%.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08841461B2uspto-grants-2014_09