反应 #1543033

ord-288b4e23f7074365a9b760c5013ec9c3

反应方程式

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

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05843416uspto-grants-1998_12