Patent ID: 9695177
Date: 2017-07-04
CPC Classifications: C06B,C07D

Claim:
1. A process for preparing tetranitroglycoluril (TNGU) via an in situ decomposition of a nitrimino group with elimination of nitrogen without the use of dinitrogen pentoxide comprising: a nitrimino moiety selected from the group consisting of N,N′-dinitrotetrahydroimidazo[4,5-d]imidazole-2,5(1H,3H)diimine, N-nitrotetrahydroimidazo[4,5-d]imidazole-2,5(1H,3H)diimine hydrochloride, and N-nitrotetrahydroimidazo[4,5-d]imidazole-2,5(1H,3H)diimine nitrate; wherein the moiety is dissolved in a from about 1 ml to about 3 ml solution of 100% nitric acid under an inert nitrogen atmosphere and at a temperature of about zero (0) degrees Celsius; wherein there is added two milliliters of a 100 percent trifluoroacetic anhydride solution drop wise at such a rate as to keep the temperature of the solution below ten (10) degrees Celsius; further wherein the solution is allowed to warm to from about 20° C. to about 26° C. with stirring for about two (2) hours until the precipitant is settled; and wherein the precipitant is washed with anhydrous dichloromethane, dried under vacuum at 10 torr with a yield of about 70.1 milligrams (0.22 mmol, 49%) of tetranitroglycoluril (TNGU).