反应 #992675

ord-5e992babb9514177bb334f7e36a2c9ad

反应方程式

O=C(O)C(=O)O
Oxalic acid
N=C(N)NN.O=C(O)O
Aminoguanidine bicarbonate
N=C(N)N.O=C(O)O
guanidine carbonate
NC(N)=[NH2+].NC(N)=[NH2+].O=C([O-])C(=O)[O-]
Guanidinium Oxalate

溶剂

反应条件

温度
90°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他to avoid bubbling over the sides of the beaker due to the evolution of carbon dioxide during the reaction
  2. 2
    workup.STIRRINGThe reaction was stirred at room temperature overnight (approximately 24 hours)
  3. 3
    其他The water was removed from the reaction mixture in vacuo
  4. 4
    其他The product was recovered as a crystalline white solid

实验过程

Oxalic acid (200.0 g, 2.22 mol) was weighed into a 2-liter beaker with a magnetic stir bar and dissolved in 1500 ml of distilled water. Aminoguanidine bicarbonate (362.8 g, 2.67 mol) and guanidine carbonate (160.1 g, 0.89 mol) were added in portions with stirring as to avoid bubbling over the sides of the beaker due to the evolution of carbon dioxide during the reaction. The reaction was stirred at room temperature overnight (approximately 24 hours). The water was removed from the reaction mixture in vacuo with heating to approximately 90° C. for 4 hours. The product was recovered as a crystalline white solid.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08012277B2uspto-grants-2011_09