ChemicalBook CAS DataBase List N,N-Bis[1(2)H-tetrazol-5-yl]amine

N,N-Bis[1(2)H-tetrazol-5-yl]amine synthesis

6synthesis methods

Product Name:N,N-Bis[1(2)H-tetrazol-5-yl]amine
CAS Number:127661-01-2
Molecular formula:C2H3N9
Molecular Weight:153.11

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Yield: 93%

Reaction Conditions:

with hydrogenchloride;sodium azide in water at 55 - 100;Reagent/catalyst;

Steps:

1
Charged 100 gm of sodium dicynamide (1.123 mol) and 153 gm of sodium azide (2.35 mol) along with water (600 ml) at room temperature, into a four neck round bottom flask fitted with mechanical stirrer, condenser, thermometer and one addition funnel.
Slowly heated the reaction mixture to 55° C. and at this temperature added 6 molar solution of hydrochloric acid (400 ml) was added into the reaction mixture for a period of 2 to 6 hour.
Then reaction mixture was heated to reflux (98° to 100° C.) for 25 hour.
After completion of the reaction, cooled the reaction mixture to 55° C. and to it was added 400 ml of 6 molar hydrochloric acid, adjusted the pH to 0.5 (<1).
Stirred the reaction mixture at the same temperature for another 1 hour.
Then cooled the reaction mixture to 25° to 30° C. or another 1 hour.
Filtered the reaction mixture, washed with water (100 ml) to get 158 gm of bis-(1(2)H-tetrazol-5-yl)-amine monohydrate (yield: 93%) having an HPLC purity of 99% without any further crystallization.

References:

IYENGAR, Deevi Sarangapani;SAIKIA, Anil;BHIMIREDDY, Nagi Reddy US2014/66630, 2014, A1 Location in patent:Paragraph 0012

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References

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References