Реакция #1528381

ord-e1876de077cb4ea28762bb59d8f524d0

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеto obtain a yellow precipitate
  2. 2
    ФильтрацияThereafter, the precipitate was collected by filtration under reduced pressure
  3. 3
    Другоеrecrystallized from a solution of DMF/water (50:50 (w/w))
  4. 4
    Другоеto give an intermediate
  5. 5
    Другоеplaced in an ice bath
  6. 6
    Другоеto obtain a precipitate
  7. 7
    ФильтрацияThe precipitate was collected by filtration under reduced pressure
  8. 8
    Другоеrecrystallized from a solution of ethanol/water (50:50 (w/w))

Методика

37.8 g (0.3 mol) of dimethylmaleic anhydride was slowly added to a solution of 41.1 g (0.3 mol) of p-aminobenzoic acid and 300 ml of acetone in a 250 ml flask at 10° C. The mixture was stirred for 2 hours to obtain a yellow precipitate. Thereafter, the precipitate was collected by filtration under reduced pressure and recrystallized from a solution of DMF/water (50:50 (w/w)) to give an intermediate. The intermediate was treated with sodium acetate and acetic anhydride at 85° C. for 4 hours, cooled to room temperature, and placed in an ice bath to obtain a precipitate. The precipitate was collected by filtration under reduced pressure and recrystallized from a solution of ethanol/water (50:50 (w/w)) to give N-(p-carboxyphenyl)dimethylmaleimide.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07655155B2uspto-grants-2010_02