Organic compounds -- part of the class 532-570 series – Organic compounds – Four or more ring nitrogens in the bicyclo ring system
Patent
1992-06-05
1993-05-18
Ford, John M.
Organic compounds -- part of the class 532-570 series
Organic compounds
Four or more ring nitrogens in the bicyclo ring system
C07D48708
Patent
active
052123081
ABSTRACT:
The invention provides a continuous moving bed reactor, useful for the prration of 3,7-diacetyl-1,3,5,7-tetraazabicyclo-3.3.1-nonane (DAPT). The reactor makes novel use of water, a known catalyst for said reaction. However, in this invention, the water is present as ice. The ice is made to automatically promote and moderate the reaction as well as regulate the flow of hexamine into the reactor. These automatic functions are achieved by mixing ice with hexamine, the latter is one of two principle reactants used, to generate a standing bed of slurry. When melted at its base, the slurry advanced under the influence of gravity. The melting of the ice being caused by local application of the second principle reactant, acetic anhydride, which is a liquid.
The apparatus is constructed in the following way. A tube shaped reservoir for containing the cited slurry is open at the top end and terminates at its bottom end by a porous compartment. The latter compartment openly retains the slurry. A fluid delivery device, i.e. a nozzle, is contained within the porous compartment. The functions of the nozzle is to deliver acetic anhydrid to the hexamine contained in said slurry.
The porous compartment is contained within a larger nonporous vessel. The vessel is equipped with a stirrer, an ammonia inlet and a temperature sensing device. This vessel functions as a secondary reaction zone, in which more hexamine, and hece more DAPT, is prepared by an in-situ mechanism commonly known as resynthesis.
REFERENCES:
patent: 3979379 (1976-09-01), Siele
patent: 4048167 (1977-09-01), Paul et al.
Alster Jack
Lukasavage William S.
Nicolich Steven M.
Portnoy Seymour
Costigan Edward
Ford John M.
Goldberg Edward
Lane Anthony T.
The United States of America as represented by the Secretary of
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