Process for the large-scale synthesis of 4,10-dinitro-2,6,8-12-t

Details Process for the large-scale synthesis of 4,10-dinitro-2,6,8-12-t Process for the large-scale synthesis of 4,10-dinitro-2,6,8-12-t

1999-07-28

2000-08-22

Lambkin, Deborah C.

Organic compounds -- part of the class 532-570 series

Organic compounds

Unsubstituted hydrocarbyl chain between the ring and the -c-...

C07D26702

Patent

active

061074837

ABSTRACT:
A process for synthesizing 4,10-dinitro-2,6,8,12-tetraoxa-4,10-diazatetracyclo-[5.5.0.0.sup.5,9 0.sup.3,11 ]-dodecane ("TEX") involves combining at least one hexa-substituted piperazine derivative with a medium containing at least one nitronium anion source and at least one acid sufficiently strong to generate nitronium anions from the nitronium anion source. According to this invention, TEX yield is significantly improved by pre-heating the medium to 55.degree. C. to about 70.degree. C. and maintaining the medium from 55.degree. C. to about 70.degree. C. to permit the hexa-substituted piperazine derivative and nitronium anions to react and form the TEX. At least one NO.sub.x scavenger is added to the medium, preferably before the addition of the hexa-substituted piperazine derivative, to increase TEX yield.

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Ramakrishnan and Boyer, "4,10-Dinitro-2,6,8,12-Tetraoxa-4,10-Diazatracyclo[5.5.0.0.sup.5,9 0.sup.3,11 ]-dodecane," Heterocycles vol. 31, pp. 479-481 (1989).

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