反応 #431803

ord-501fb714cc924c2fb5fb0d9fc22033e4

反応方程式

CCCCCCCCCCCC(=O)[O-].CCCCCCCCCCCC(=O)[O-].CCC[CH2][Sn+2][CH2]CCC
dibutyltin dilaurate
O=[N+]([O-])Nc1nnn[nH]1.[NH4+]
ammonium 5-nitraminotetrazole
N[NH+]=C(N)N(N)N.O=[N+]([O-])Nc1nnn[nH]1
triaminoguanidinium 5-nitraminotetrazole
N1=NC(=C2N=NN=N2)N=N1
5,5'-bitetrazole
NNC(N)=[NH2+].O=C([O-])O
aminoguanidinium bicarbonate
N1=NC(=C2N=NN=N2)N=N1.NNC(N)=[NH2+]
aminoguanidinium 5,5'-bitetrazole

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONThe high nitrogen content solid is then added
  2. 2
    その他to form a uniform suspension
  3. 3
    その他Aminoguanidinium 5,5'-bitetrazole is synthesized
  4. 4
    ろ過The solution is filtered while hot and the filtrate
  5. 5
    温度rapidly chilled in an ice bath
  6. 6
    ろ過The product is filtered off
  7. 7
    洗浄washed twice with cold water and vacuum
  8. 8
    その他dried at 70° C.

実験手順

The high nitrogen content solid is then added to form a uniform suspension. A catalyst such as dibutyltin dilaurate is also used. The solids ammonium 5-nitraminotetrazole and triaminoguanidinium 5-nitraminotetrazole, are synthesized by known methods. Aminoguanidinium 5,5'-bitetrazole is synthesized by dissolving 5,5'-bitetrazole (12.7g) and aminoguanidinium bicarbonate (12.5g) in boiling water (160 ml). The solution is filtered while hot and the filtrate rapidly chilled in an ice bath. The product is filtered off, washed twice with cold water and vacuum dried at 70° C., 25 mm to give a 91% (17.8g) yield of aminoguanidinium 5,5'-bitetrazole. The solid guanidinium 5,5'-bitetrazole is synthesized by adding a filtered solution of guanidinium bicarbonate (9.0g, 0.05 mole) in boiling water (75 ml) to a filtered boiling solution of 5,5'-bitetrazole (13.8g, 0.1 mole) in water (200 ml). The resulting solution is cooled rapidly in an ice-water bath. The white, crystalline product is removed by filtration, washed once with cold water and vacuum dried at 70° C., 25 mm to give a 95.6% (18.8g) yield of guanidinium 5,5'-bitetrazole.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05053086uspto-grants-1991_10