Starting from tetraacetyldibenzy-lhexaazaisowurtzitane (TADBIW), tetraacetylhexaazaisowurtzitane（TAIW）was synthesized via catalytic hydrigenolysis debenzylation using palladium compound as catalyst. Tetraacetyl-bis- (4-chlorobenzoyl)hexaazaisowurtzitane (TABIW) was synthesized through reaction of the condensation of TAIW and 4-chlorobenzoyl chloride. Finally the title compound tetranitro-bis(3,5-dinitro-4-chloroben- zoyl)hexaazaisowurtzitane (TNBIW) was obtained by the nitration of TABIW with oleum（w(SO₃)=20%）/ fuming nitric acid （w(HNO₃) =98%）at 90 ℃ for 4 h. The melting point of TNBIW is 242-244 ℃, and its yield is 57.2%（based on the numbers of TADB）. The structures of TNBIW and its two intermediates were (TABIW, TAIW） determined by IR, 1HNMR, MS and elemental analysis.