تفاعل #1543033

ord-288b4e23f7074365a9b760c5013ec9c3

معادلة التفاعل

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

الكواشف

لا شيء

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

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

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05843416uspto-grants-1998_12