3,5-dinitro-1H-1,2,4-triazole → sodium tetrakis(3,5-dinitro-1H-1,2,4-triazolyl)borate

関与物質

反応条件

反応手順

Under anhydrous conditions and a stream of dry nitrogen, 6.36 g (40.0 mmol) 3,5-dinitro-1H-1,2,4-triazole and 37.8 mg (10.0 mmol) sodium borohydride were loaded into a dry 250 mL three-necked round bottom flask that was equipped with a TEFLON™ coated stirring bar, an addition funnel and a reflux condenser. While stirring, 50 mL of anhydrous 1-methoxy-2-(2-methoxyethoxy)ethane (diglyme) was carefully added through the addition funnel. Immediately, hydrogen gas was evolved and the reaction mixture turned yellow-orange. When the addition was complete, the addition funnel was replaced by a stopper. The mixture was heated to 50° C. for three hours and then to 110° C. for an additional 24 hours. The obtained orange solution was allowed to cool to ambient temperature and all volatiles were pumped-off in vacuo. Subsequent evacuation to a constant weight over a period of 48 hours resulted in a yellow solid of sodium tetrakis(3,5-dinitro-1H-1,2,4-triazolyl)borate, 8.5 g. Decomposition temperature: 167.6° C. (TGA, weight loss: 69.4%), density: 1.80 g/cm3 at 20° C.

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