Reaction #1543033

ord-288b4e23f7074365a9b760c5013ec9c3

Conditions

Detailed conditions
See reaction.notes.procedure_details.

Workup

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

Procedure

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.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05843416uspto-grants-1998_12