참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 3,5-dinitro-1H-1,2,4-triazole | HCID 3283598 | — |
| 반응물 | Sodium borohydride | HCID 4311764 | — |
| 반응물 | HCID 178418361 | HCID 178418361 | — |
| 용매 | Diglyme | HCID 8150 | — |
| 생성물 | sodium tetrakis(3,5-dinitro-1H-1,2,4-triazolyl)borate | HCID 131735306 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09309266B2 |
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| 출처 데이터셋 | uspto-grants-2016_04 |
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| ORD ID | ord-29b5eb4f4eaf492895480b444328247c |
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| 출처 메모 | uspto-grants-2016_04 |
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