反应详情

温度

-196 °C

A 150 mL glass ampule equipped with a grease-free high-vacuum PTFE valve and a TEFLON™ coated stir bar was flamed-out under vacuum. Inside the dry-box, the ampule was loaded with 588 mg (4.00 mmol) 3,5-dinitro-1H-1,2,4-triazole and 53.9 mg (1.00 mmol) potassium borohydride. The ampule was connected to a vacuum line, evacuated and cooled to −196° C. About 5 mL of dry dimethoxyethane was slowly condensed into the ampule. The ampule was closed and allowed to warm to ambient temperature. As soon as the solvent melted and contacted the solid mixture at the bottom of the ampule, gas evolution started. The mixture was then stirred for about 30 minutes at ambient temperature. The clear, light yellow solution was cooled to −196° C., and 1.5 mmol of evolved hydrogen (determined by p, V, T measurements) were pumped off. The ampule was closed off and heated to 60° C. while stirring. After 3 hours, an orange solution was obtained and the temperature was first raised to 80° C. and, after an additional 8 hours, to 110° C. After 24 hours, the solution was allowed to cool to ambient temperature and then cooled to −196° C. An additional 2.50 mmol of evolved hydrogen (determined by p, V, T measurements) was pumped off. The reaction mixture was allowed to warm to ambient temperature. Subsequent evacuation to a constant weight over 24 hours resulted in an orange solid of potassium tetrakis(3,5-dinitro-1H-1,2,4-triazolyl)borate, 1.0 mmol. Decomposition temperature: 165° C. (DTA).

1. customevacuated
2. customcondensed into the ampule
3. customThe ampule was closed
4. temperatureto warm to ambient temperature
5. temperatureThe clear, light yellow solution was cooled to −196° C.
6. customThe ampule was closed off
7. temperatureheated to 60° C.
8. stirringwhile stirring
9. waitAfter 3 hours
10. customan orange solution was obtained
11. temperaturethe temperature was first raised to 80° C. and, after an additional 8 hours, to 110° C
12. waitAfter 24 hours
13. temperatureto cool to ambient temperature
14. temperaturecooled to −196° C
15. temperatureto warm to ambient temperature