Реакция #9863

ord-9a87187d185b4d9390fcb9daeac9bc76

Растворители

Условия реакции

Температура
150°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеThe solvent (DMF) was removed on the rotovap under high vacuum at 90° C
  2. 2
    workup.ADDITIONThe residue was diluted with 600 mL of aqueous citric acid (5%)
  3. 3
    Температураcooled to 0° C.
  4. 4
    ФильтрацияThe tan powder was filtered
  5. 5
    Другоеdried overnight

Методика

2-Amino-thiophene-3-carboxlic acid amide (28.4 g, 0.2 mol) and potassium ethylxanthate (96 g, 3 eq) were mixed together and added to DMF (1000 mL). The resulting mixture was heated to 150° C. for about six hours. The solvent (DMF) was removed on the rotovap under high vacuum at 90° C. The residue was diluted with 600 mL of aqueous citric acid (5%) and cooled to 0° C. and stirred for about 30 minutes. The tan powder was filtered and dried overnight to give 25.6 g of the title compound ((M+H)+=185, M.P.>300° C.).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07091347B2uspto-grants-2006_08