Preparation and Purification of HMX and RDX Intermediates (TAX and SEX).
Final rept. 1 Dec 79-30 Apr 80,
SRI INTERNATIONAL MENLO PARK CA ORGANIC CHEMISTRY DEPT
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This report describes the feasibility of preparing 4 kg each of 1-acetylhexahydro-3.5-dinitro-1,3,5-triazine TAX and 1-acetyloctahydro-3,5,7-trinitro-1,3,5,7-tetrazocine SEX. TAX was prepared by nitrolysis of 1,3,5-triacetylhexahydro-1,3,5-triazine TRAT using a mixture of trifluoroacetic anhydride TFAA and 100 nitric acid. The crude TAX, contaminated with 5 to 30 RDX, was obtained analytically pure 99.9 by open column chromatography on silica gel using a 11 mixture of nitromethanedichloromethane as eluent. SEX was prepared by nitrolysis of 1,5-diacetyloctahydro-3,7-dinitro-1,3,5,7-tetrazocine DADN using a mixture of trifluoroacetic anhydride and 100 nitric acid. The crude SEX was contaminated with 50 DADN, HMX, or both, depending on the reaction conditions. Soxhlet extraction of the crude SEX with ethyl acetate affords 80 SEX with 20 DADN contaminated. Because the major problem is not the synthesis of SEX but its purification, additional methods for purification and further examination of solvent systems used for extractive and chromatographic separations should be explored to obtain analytically pure SEX.
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