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Ammonia;borane → ammonium tetrakis(5-(trinitromethyl)-2H-tetrazolyl)borate

HRID 627301
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HRID 627301 반응식
[N+:1]([C:4]([N+:13]([O-:15])=[O:14])([N+:10]([O-:12])=[O:11])[C:5]1[N:6]=[N:7][NH:8][N:9]=1)([O-:3])=[O:2].[NH3:16].[BH3:17].[H][H]>>[N+:13]([C:4]([N+:1]([O-:3])=[O:2])([N+:10]([O-:12])=[O:11])[C:5]1[N:6]=[N:7][N:8]([B-:17]([N:7]2[N:8]=[N:9][C:5]([C:4]([N+:1]([O-:3])=[O:2])([N+:10]([O-:12])=[O:11])[N+:13]([O-:15])=[O:14])=[N:6]2)([N:7]2[N:8]=[N:9][C:5]([C:4]([N+:1]([O-:3])=[O:2])([N+:10]([O-:12])=[O:11])[N+:13]([O-:15])=[O:14])=[N:6]2)[N:16]2[N:8]=[N:9][C:5]([C:4]([N+:13]([O-:15])=[O:14])([N+:1]([O-:3])=[O:2])[N+:10]([O-:12])=[O:11])=[N:6]2)[N:9]=1)([O-:15])=[O:14].[NH4+:1]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 419330Ammonia;boraneHCID 109550355-(trinitromethyl)-2H-tetrazoleHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 131735314ammonium tetrakis(5-(trinitromethyl)-2H-tetrazolyl)borate

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온도
-196 °C

실험 절차

A 100 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 896 mg (4.00 mmol) 5-(trinitromethyl)-2H-tetrazole and 30.8 mg (1.00 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 100° C. for eight hours. The obtained yellow solution was cooled to −196° C. and the 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(5-(trinitromethyl)-2H-tetrazolyl)borate, 4.0 mmol.

후처리

  1. customevacuated
  2. customcondensed into the ampule
  3. customThe ampule was closed
  4. temperatureto warm to ambient temperature
  5. temperaturethe ampule was heated to 100° C. for eight hours
  6. temperatureThe obtained yellow solution was cooled to −196° C.
  7. temperatureto warm to ambient temperature

출처 및 근거

ORD 기록
ord-8d6007f2e18e4cc489ad20591e2c4892
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09309266B2

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