반응 #431803
ord-501fb714cc924c2fb5fb0d9fc22033e4
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후처리
- 1workup.ADDITIONThe high nitrogen content solid is then added
- 2기타to form a uniform suspension
- 3기타Aminoguanidinium 5,5'-bitetrazole is synthesized
- 4여과The solution is filtered while hot and the filtrate
- 5온도rapidly chilled in an ice bath
- 6여과The product is filtered off
- 7세척washed twice with cold water and vacuum
- 8기타dried at 70° C.
실험 절차
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.