Synthetic method of hexabenzylhexaazaisowurtzitane

A technology of hexabenzyl hexaazide and isowurtzitane is applied in the field of synthesis of hexabenzyl hexaaz isowurtzitane, and can solve the problems of affecting product quality and yield, loss of amino nucleophilic ability, etc. The effect of reducing side reactions and improving application efficiency

Inactive Publication Date: 2010-01-13
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Claims
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Problems solved by technology

Therefore, the hydrogen ions in the catalyst acid can combine with the carbonyl group to form salt to increase the electrophilicity of the carbonyl group, and at the same time, it can combine with the amino group to form an ammonium salt and lose the nucleophilic ability of the amino group, see formula (2), (3), this reaction is a side reaction of the HBIW condensation reaction, affecting the quality of the product and yield

Method used

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  • Synthetic method of hexabenzylhexaazaisowurtzitane
  • Synthetic method of hexabenzylhexaazaisowurtzitane
  • Synthetic method of hexabenzylhexaazaisowurtzitane

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Embodiment 1

[0026] 4.4 liters of acetonitrile, 0.44 liters of distilled water, and 480 g of benzylamine were added to a 12-liter reaction vessel, and stirred. 292 grams of 40% glyoxal aqueous solution and 23.2 g of formic acid (88% by weight) were thoroughly mixed, and slowly added to the reaction system with a constant pressure dropping funnel for 2.5 hours. The constant pressure dropping funnel was washed with distilled water, and the washing water was also added to the reaction flask. After the addition was complete, the stirring reaction was continued at room temperature for 24 h, and finally the reactant was filtered. The HBIW crude product has a purity of 81.1% (HPLC purity), and a yield of 82.6% by weight (the ratio of the weight of the product actually obtained to the theoretical amount calculated from the amount of glyoxal).

Embodiment 2

[0030] Method is the same as Example 1, except that the acid catalyst used is hydrochloric acid.

Embodiment 3

[0034] Method is the same as Example 1, except that the acid catalyst used is p-toluenesulfonic acid.

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Abstract

The invention relates to a preparation method of initial intermediate hexabenzylhexaazaisowurtzitane of a high energy density compound HNIW, comprising the following steps: (1) mixing a solvent with benzylamine and placing the mixture into a reactor; (2) mixing acid catalysts with a glyoxal water solution to prepare an aldehydic acid mixed solution; (3) slowly adding the prepared aldehydic acid mixed solution into the reactor and stirring for reaction; and (4) after dripping the aldehydic acid mixed solution, continuously stirring for reaction until the reaction is completely finished, and then separating to obtain hexabenzylhexaazaisowurtzitane solid products.

Description

technical field [0001] The invention relates to a synthesis method of hexabenzylhexaazowurtzitane, which relates to the field of explosives. Background technique [0002] Hexabenzylhexaazaisowurtzitane (HBIW) is the initial intermediate for the synthesis of high energy density compound hexanitrohexaazaisowurtzitane (HNIW), in 1990 Nielsen A T et al. 2. Formation of 2, 4, 6, 8, 10, 12-hexabenzyl-2, 4, 6, 8, 10, 12-hexaazatetracycle[5.5.0.0 5.9 .0 3.11 ]dodecanesfrom glyoxal and benzylamines reported the synthesis of HBIW, that is, using acetonitrile as the reaction medium, formic acid as the catalyst, adding benzylamine and glyoxal at room temperature to obtain HBIW, the yield is about 80% (such as formula 1). If methanol is used instead as the intermediate reactant, the yield is lower (64%). Using 95% ethanol as the reaction medium, the product yield is lower than that of acetonitrile as the reaction medium. At present, the synthesis reaction of HBIW adopted both at hom...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/22
Inventor 金韶华李丽洁刘进全陈华雄陈树森史彦山
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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