Reacción #1543033

ord-288b4e23f7074365a9b760c5013ec9c3

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otrowas kept below or equal to 30° C
  2. 2
    workup.STIRRINGStirring
  3. 3
    OtroA slight cloudiness was removed by filtration on sintered glass
  4. 4
    OtroThe filtrate was evaporated to dryness at reduced pressure
  5. 5
    OtroThe solid obtained
  6. 6
    Otrowas recrystallized from ethyl acetate
  7. 7
    FiltraciónAfter filtering
  8. 8
    Otrodrying in vacuum at 50° C.

Procedimiento

31 g of methyl ester of N-(2-mercapto-ethyl)malonamic acid obtained in Example 3a) were added to 220 cm3 of aqueous 20% solution of aqueous ammonia, with stirring, while the temperature was kept below or equal to 30° C. Stirring was continued for 1 hour at ambient temperature. A slight cloudiness was removed by filtration on sintered glass. The filtrate was evaporated to dryness at reduced pressure. The solid obtained was recrystallized from ethyl acetate. After filtering and drying in vacuum at 50° C., 27 g of N-(2mercaptoethyl)malonamide were obtained in the form of a white solid with a melting point of 100° C.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05843416uspto-grants-1998_12