Réaction #2298618

ord-32c3794161204a7eb2dd3faa7b51ab85

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Températurewhile cooling in an ice bath
  2. 2
    AutreThe cooling bath was removed
  3. 3
    workup.ADDITIONThe reaction mixture was diluted with water (100 mL)
  4. 4
    Filtrationthe solid product collected by vacuum filtration

Mode opératoire

Formic acid (40 mL) was added to acetic anhydride (60 mL) while cooling in an ice bath. Solid 3-amino-2-thiophenecarboxylic acid methyl ester (77, 10.3 g, 66 mmol) was added to the cold solution in small portions. The cooling bath was removed and the resulting suspension was stirred at room temperature for 4 hours. The reaction mixture was diluted with water (100 mL) and the solid product collected by vacuum filtration to yield 3-(formylamino)-2-thiophenecarboxylic acid methyl ester (10.3 g, 85% yield) as a white solid.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: USRE039267E1uspto-grants-2006_09