반응 #1543033

ord-288b4e23f7074365a9b760c5013ec9c3

반응 방정식

O=C(O)CC(=O)NCCS
N-(2-mercapto-ethyl)malonamic acid
N
ammonia
NC(=O)CC(=O)NCCS
N-(2mercaptoethyl)malonamide

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

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

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05843416uspto-grants-1998_12