Preparation and Purification of HMX and RDX Intermediates (TAX and SEX).
Abstract
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 1:1 mixture of nitromethane/dichloromethane 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.
Document Details
- Document Type
- Technical Report
- Publication Date
- May 01, 1980
- Accession Number
- ADA089613
Entities
People
- Clifford D. Bedford
- Donald L. Ross
- Maria A. Geigel
- Steven J. Staats
Organizations
- SRI International