Patent ID: 6512113
Filing Date: 2003-01-28
Classification: C06B,C07D

Abstract:
A process for preparing 4,10-dinitro-2,6,8,12-tetraoxa-4,10-diazatetracyclo[5.5.0.05,903,11]-dodecane by reacting at least one hexa-substituted piperazine derivative with at least one nitrate source, the reaction between the hexa-substituted piperazine and the nitrate source being characterizable by sequentially having an initial stage which is highly exothermic so that a cooling source is needed to maintain the reaction below about 80Â° C., an intermediate stage which is substantially non-exothermic so that the cooling source is not needed to maintain the reaction below about 80Â° C., and a NOx autocatalytic stage in which gases comprising NOx are generated autocatalytically and exothermically, said process comprising;(a) combining the hexa-substituted piperazine derivative with a medium comprising the nitrate source and optionally at least one strong acid and heating the medium to a temperature sufficient to induce the initial stage of the reaction between the hexa-substituted piperazine derivative and the nitrate source; (b) maintaining the medium at a temperature in a range of at least ambient to not more than about 80Â° C. during the initial stage and at least a portion of the intermediate stage of the reaction by cooling the medium during at least a portion of the initial stage of the reaction so that the reaction proceeds in a controlled manner; and (c) cooling the medium prior to the NOx autocatalytic stage to about 0Â° C. to prevent commencement of the exothermic NOx autocatalytic stage.