The benzyl groups of monoacetyltribenzoyldibenzylhexaazaisowutzitane were removed successfully by the nitrosification of 65% HNO₃/NaNO₂. And the corresponding nitrosamine product—monoacetyltribenzoyldinitrosohexaazaisowutzitane was obtained. Using thin-layer chromatography(TLC) and column chromatography (CC) methods,two kinds of by-products of the nitrosation products from monoacetyltribenzoyldibenzylhexaazaisowutzitane were isolated and identified as monoacetyltetrabenzoylmononitrosohexaazaisowutzitane and monoacetylpentabenzoylhexaazaisowutzitane.