反应 #3740

ord-12e40ee7e23541c4b9a7cdf8dcd80cd1

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度was heated
  2. 2
    温度under reflux for 0.75 hour
  3. 3
    温度to cool
  4. 4
    其他The solid which precipitated
  5. 5
    过滤was collected by filtration
  6. 6
    其他crystallised from methanol

实验过程

A mixture of 2-amino-2-cyanoacetamide (2.8 g, 0.0282 mol), trimethylorthoformate (3.4 g, 0.0321 mol) and acetonitrile (55 ml) was heated under reflux for 0.75 hour, then allowed to cool. n-Propylamine (1.8 g, 0.0305 mol) was then added dropwise, and the resulting mixture stirred at ambient temperature for 36 hours. The solid which precipitated was collected by filtration and crystallised from methanol to give the title compound as a colourless solid (2.9 g, 61%), m.p. 241°-243° C. Found: C,49.67; H,7.15; N,33.64. C7 H12N4O requires C,49.98; H,7.19; N,33.31%.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05734053uspto-grants-1998_03