Preparation and Purification of Multigram Quantities of TAX and SEX.
Abstract
This final report describes the multigram preparation and purification of l-acetylhexahydro-3,5-dinitro-l,3,5-triazine (TAX) and the feasibility of preparing, purifying, and analyzing multigram quantities of l-acetyloctahydro-3,5,7-trinitro-1,3,5,7-tetr azocine (SEX) needed for toxicological testing. 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. A continuous plug-flow reactor design was found to be a rapid, efficient, and safe method for the preparation of TAX in kilogram quantities. The crude TAX, contaminated with 25% to 30% RDX, was obtained analytically pure (99.9+%) by high-pressure liquid chromatography (HPLC) on silica gel using nitromethane as the eluent. SEX was prepared by nitrolysis of 1,5-diacetyloctahydro-3,7-dinitro-1,3,5,7-tetrazocine (DADN), using a mixture of 30% oleum and 100% nitric acid. Conditions for the preparation of the DADN/SEX/HMX mixture were optimized and the process can be conducted batchwise. Thus SEX could be provided in the quantities desired for subsequent purification.
Document Details
- Document Type
- Technical Report
- Publication Date
- Dec 01, 1981
- Accession Number
- ADA122816
Entities
People
- Bruce D. Deas
- Clifford D. Bedford
- Majorie M. Broussard
- Maria A. Geigel
Organizations
- SRI International