FIELD: organic chemistry, chemical technology.
SUBSTANCE: invention relates to a method for preparing an intermediate substance tetraacetyldiformylhexaazaizowurtzitane used in preparing highly effective explosive substance 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazatetracyclo[5,5,0,03,11,05,9]dodecane. Invention describes a method for preparing 4,10-diformyl-2,6,8,12-tetraacetyl-2,4,6,8,10,12-hexaazatetracyclo[5,5,0,03,11,05,9]dodecane by hydrogenolysis of 4,10-dibenzyl-2,6,8,12-tetraacetyl-2,4,6,8,10,12-hexaazatetracyclo[5,5,0,03,11,05,9]dodecane in formic acid medium and water to form toluene as a by-side product followed by removal of formic acid, water and toluene from the reaction mass by using azeotropic distillation off with benzene or toluene at temperature lower formic acid boiling point. Formed azeotrope is cooled, benzene or toluene is recovered to the process and prepared product is crystallized in medium of two successively added organic solvent wherein one solvent homogenizes the reaction mass and another solvent precipitated the prepared product, for example, ethanol and ethyl acetate, or ethanol and isopropanol, or acetone and ethyl acetate, or acetone and isopropanol, or methanol and isopropanol.
EFFECT: improved preparing method.
2 cl, 2 tbl, 3 ex
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Authors
Dates
2005-12-27—Published
2003-08-25—Filed