Process for the preparation of 5,5'-bi-1H-tetrazole salt

Details Process for the preparation of 5,5'-bi-1H-tetrazole salt Process for the preparation of 5,5'-bi-1H-tetrazole salt

1999-08-16

2000-12-05

McKane, Joseph

Organic compounds -- part of the class 532-570 series

Organic compounds

Heterocyclic carbon compounds containing a hetero ring...

C07D25704, C07D40304

Patent

active

061569062

ABSTRACT:
A process for the preparation of a 5,5'-bi-1H-tetrazole diammonium salt by dropwisely adding the aqueous hydrogen peroxide to which a small amount of weakly acidic substance has been added, to a starting aqueous solution containing hydrogen cyanide or sodium cyanide or potassium cyanide, sodium azide and a catalytic amount of copper sulfate preferably at a low temperature to maintain the pH of the reaction solution over a range of from 5 to 6, heating the reaction solution to effect the oxidation and cyclization reaction, reacting the reaction product with ammonium chloride or an aqueous solution thereof, and recovering the formed ammonium salt in the form of sparingly soluble crystals. The desired product is obtained in a high yield and in a high purity from the starting materials which are cheaply available and are easy to handle through a decreased number of steps, i.e., through a one-pot reaction without requiring cumbersome after-treatment.

REFERENCES:
Fred Einberg, "Preparatioon of 5-Dinitromethyletrazole from Salts of Dinitroacetonitrile", Journal of Organic Chemistry, vol. 29, -1964, pp. 2021-2024, XP002135258.
American Chemical Society. Easton., US ISSN: 0022-3263, p. 2023, left column.

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