Patent ID: 9056868
Filing Date: 2015-06-16
Classification: C07D

Abstract:
1. A method for making CL-20, comprising: preparing hexa(arylmethyl)hexaazaisowurtzitane (A) wherein arylmethyl is selected from the group consisting of 2-naphthylmethyl, 1-naphthylmethyl, 9-anthracenylmethyl, and any combination thereof dissolving said hexa(arylmethyl)hexaazaisowurtzitane in at least one dipolar aprotic solvent and treating with at least one aliphatic anhydride, at least one heterogeneous hydrogenation catalyst, and hydrogen gas while in a closed reaction vessel to form a solution which is allowed to react with heating; removing said heterogeneous hydrogenation catalyst by filtration to afford a filtrate solution; isolating TADA (B) from said filtrate solution by addition of at least one non-solvent; treating said TADA with concentrated nitric acid and isolating crude CL-20 by dilution with water and collecting said CL-20 by filtration; recrystallizing of said CL-20 by suspension in a solvent mixture having saturated poly alpha-olefins (PAO), and a three solvent system, removing at least one of said solvent under reduced-pressure while heating; cooling said solution to about 25° C. to about 30° C.; and collecting by filtration to afford about 50-200 micron size crystals of epsilon-CL-20 (C)