USA As Represented by Secretary of the Navy

Patrick A Caruana

Alfred G Stern

Michael D Williams

John William Fronabarger

Bradley Sleadd

Alex J Zaita

Thao Vo

A synthesis for an azo intermediate, 5,5'-azobis(4-chloropyrimidine) is disclosed. 5,5&#x2032;-azobis(4-chloropyrimidine) is a relatively stable azo compound in that decomposition does not occur until about 194&#xb0; C. 5,5&#x2032;-azobis(4-chloropyrimidine) is a product of oxidative dimerization of 5-amino-4-pyrimidine, which a water soluble compound. The azo intermediate is formed in an aqueous solution, but the azo intermediate is substantially insoluble in water; and as it forms it separates producing a reaction mixture that is a slurry. The azo intermediate is isolated by filtration. The azo intermediate is marginally soluble in acetone. The yield is at least 18%, and the oxidizing agent (bleach) is inexpensive, reaction conditions do not require extreme heat or cold, which taken together make the azo intermediate suitable for scaling up.

Synthesis of AZO intermediate

A batch reactor process for the synthesis of potassium 5,7-dinitro-[2,1,3]-benzoxadiazol-4-olate-3-oxide (KDNP) from 3-bromo-2,4,6-trinitroanisole (ETNA) includes adding BTNA to a reaction vessel containing potassium azide (KN) and water (HO). The resulting mixture is heated to 90&#xb0; C. followed by cooling to room temperature and agitating the final solution. The precipitate KDNP product is recovered by filtration.

Single reaction vessel process for synthesis of salts of DNP

Substituted tetraazapentalenes have two benzenoid rings and eight substitutable positions. Substitutions are made of hydrogen or C&#x2014;H groups in favor of amino groups, nitro groups or nitrogen atoms. The tetraazapentalenes are synthesized through an intermediate azo, which is made from a 1:1:1 molar ratio of a nitroaniline, sodium nitrite and an amine.

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La Plata, MD, United States of America

Patrick A Caruana