Ammonia;borane → ammonium tetrakis(3,5-dinitro-1H-1,2,4-triazolyl)borate

HRID 627298

反応式

HRID 627298 の反応式
[N+:1]([C:4]1[N:8]=[C:7]([N+:9]([O-:11])=[O:10])[NH:6][N:5]=1)([O-:3])=[O:2].[NH3:12].[BH3:13].[H][H]>>[N+:1]([C:4]1[N:8]=[C:7]([N+:9]([O-:11])=[O:10])[N:6]([B-:13]([N:5]2[C:4]([N+:1]([O-:3])=[O:2])=[N:8][C:7]([N+:9]([O-:11])=[O:10])=[N:6]2)([N:5]2[C:4]([N+:1]([O-:3])=[O:2])=[N:8][C:7]([N+:9]([O-:11])=[O:10])=[N:6]2)[N:12]2[C:7]([N+:9]([O-:11])=[O:10])=[N:8][C:4]([N+:1]([O-:3])=[O:2])=[N:5]2)[N:5]=1)([O-:3])=[O:2].[NH4+:1]

参加物

4

反応物 3

HCID 419330Ammonia;boraneHCID 32835983,5-dinitro-1H-1,2,4-triazoleHCID 178418361HCID 178418361、化合物

生成物 1

HCID 131735309ammonium tetrakis(3,5-dinitro-1H-1,2,4-triazolyl)borate

反応条件

温度
-196 °C

実験手順

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 1.18 g (8.00 mmol) 3,5-dinitro-1H-1,2,4-triazole and 61.6 mg (2.00 mmol) ammonia borane. The ampule was connected to a vacuum line, evacuated and cooled to −196° C. About 10 mL of dry dimethoxyethane was slowly condensed into the ampule. The ampule was closed and allowed to warm to ambient temperature. After 30 minutes, the ampule was heated to 110° C. for eight hours. The obtained yellow solution was cooled to −196° C. and 5.9 mmol of evolved hydrogen was pumped off. The reaction mixture was allowed to warm to ambient temperature. Subsequent evacuation to a constant weight over 24 hours resulted in a yellow solid of ammonium tetrakis(3,5-dinitro-1H-1,2,4-triazolyl)borate, 8.0 mmol.

後処理

  1. customevacuated
  2. customcondensed into the ampule
  3. customThe ampule was closed
  4. temperatureto warm to ambient temperature
  5. temperaturethe ampule was heated to 110° C. for eight hours
  6. temperatureThe obtained yellow solution was cooled to −196° C.
  7. temperatureto warm to ambient temperature

出典と根拠

ORDレコード
ord-c997c99103954c89aa5d9e746257d31c
出典データセット
uspto-grants-2016_04
特許番号
US09309266B2

関連ノート

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