反応 #514365

ord-2ddbeaa9cf7b4e8da7dd44bf9c41cde8

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.WAITWithin a few seconds
  2. 2
    洗浄The precipitate were washed with water
  3. 3
    その他dried at 50° C
  4. 4
    その他2.6 g 1,1-diamino-2,2-dinitroethylene was recovered (35% yield)

実験手順

Finely ground 2-methyl-4,5pyrimidindione (5.1 g, 0.05 mole) was dissolved in concentrated sulphuric acid (40 ml, 1.84 g/cm3) at 15-20° C. during vigorous stirring. At the same temperature nitric acid (8.0 ml, 1.52 g/cm3) was added over a 30-min period. After 3 h, the reaction mixture was poured into water. Within a few seconds, bright yellow crystals settled out (1,1-diamino-2,2-dinitroethylene). The precipitate were washed with water and dried at 50° C. 2.6 g 1,1-diamino-2,2-dinitroethylene was recovered (35% yield).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06312538B1uspto-grants-2001_11