Preparation and Purification of HMX and RDX Intermediates (TAX and SEX).
Final rept. 15 Jul 80-30 Nov 80 on phase 2,
SRI INTERNATIONAL MENLO PARK CA ORGANIC CHEMISTRY DEPT
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This final report describes the feasibility of preparing 4 kg of 1-acetyloctahydro-3,5,7-trinitro-1,3,5,7-tetrazocine SEX. The objectives were to establish the technical feasibility of producing amounts of SEX needed for toxicological testing about 4 kg, provide this material in satisfactory purity and with proper analytical characterization of residual impurities, and provide a cost-plus-fixed-fee estimate for preparation of the compound. SEX was prepared by nitrolysis of 1,5-diacetyloctahydro-3,7-dinitro-1,3,5,7-tetrazocine DADN, using a mixture of trifluoracetec anhydride and 100 nitric acid. The crude SEX was contaminated with 50 of DADN, HMX, or of a mixture of both, depending on the reaction conditions. Analytically pure SEX 99.9 was obtained through the following procedure. Open hot column chromatography 90-100 C on silica gel with a nitromethane eluent was used to remove the 5 to 20 DADN contamination. The resulting SEXHMX mixture was separated to yield 99. SEX by preparative high-pressure liquid chromatography HPLC on prepacked silica gel columns, again using a nitromethane eluent. Conditions for the preparation of the DADNSEXHMX mixture have been optimized and the process can be conducted batchwise. Thus, SEX can be provided in the quantities desired for subsequent purification. Determination of the shock sensitivity of SEX showed that it can sustain greater than 300 kg-cm in a drop weight test compared with 148 kg-cm for pure HMX. However, SEX is sensitive to direct, strong hammer blows and therefore must be treated as an explosive material in handling and shipping. Author
- Ammunition and Explosives