تفاعل #165885

ord-b659c56f7db54725a1a56263bd05b943

المذيبات

ظروف التفاعل

درجة الحرارة
130°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwas then added
  2. 2
    درجة الحرارةby heating
  3. 3
    درجة الحرارةto reflux for one hour
  4. 4
    أخرىThe resultant reaction mixture
  5. 5
    درجة الحرارةto cool
  6. 6
    أخرىby collecting the precipitated crystal
  7. 7
    ترشيحby filtration at 30° C.
  8. 8
    أخرىlower before drying under reduced pressure

الإجراء التجريبي

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%.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08841461B2uspto-grants-2014_09