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

HRID 627297Notes

Reaction equation

HRID 627297 reaction equation
[N+:1]([C:4]1[N:8]=[C:7]([N+:9]([O-:11])=[O:10])[N:6]([B-:12]([N:35]2[C:39]([N+:40]([O-:42])=[O:41])=[N:38][C:37]([N+:43]([O-:45])=[O:44])=[N:36]2)([N:24]2[C:28]([N+:29]([O-:31])=[O:30])=[N:27][C:26]([N+:32]([O-:34])=[O:33])=[N:25]2)[N:13]2[C:17]([N+:18]([O-:20])=[O:19])=[N:16][C:15]([N+:21]([O-:23])=[O:22])=[N:14]2)[N:5]=1)([O-:3])=[O:2].[Na+].[NH4+:47]>C(#N)C>[N+:43]([C:37]1[N:38]=[C:39]([N+:40]([O-:42])=[O:41])[N:35]([B-:12]([N:24]2[C:28]([N+:29]([O-:31])=[O:30])=[N:27][C:26]([N+:32]([O-:34])=[O:33])=[N:25]2)([N:13]2[C:17]([N+:18]([O-:20])=[O:19])=[N:16][C:15]([N+:21]([O-:23])=[O:22])=[N:14]2)[N:6]2[C:7]([N+:9]([O-:11])=[O:10])=[N:8][C:4]([N+:1]([O-:3])=[O:2])=[N:5]2)[N:36]=1)([O-:45])=[O:44].[NH4+:47]

Participants

4

Reactant 2

HCID 223AmmoniumHCID 131735306sodium tetrakis(3,5-dinitro-1H-1,2,4-triazolyl)borate

Product 1

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

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent

Procedure

A solution of 10.0 g (15.0 mmol) sodium tetrakis(3,5-dinitro-1H-1,2,4-triazolyl)borate in 100 mL anhydrous acetonitrile was passed through a column containing 30 g (135 meq) of the anhydrous ammonium loaded Amberlyst-15 ion-exchange resin and the eluent collected in a 500 mL Schlenk flask. The column was washed with an additional 100 mL of anhydrous acetonitrile. Subsequent evacuation of the vessel containing the combined yellow eluents to a constant weight over 24 hours resulted in a yellow, glass-like solid of ammonium tetrakis(3,5-dinitro-1H-1,2,4-triazolyl)borate, 14.5 mmol. Decomposition temperature: 173.8° C. (DTA onset), 177.8° C. (TGA, weight loss: 86.4%) density: 1.73 g/cm3 at 20° C.

Workup

  1. customthe eluent collected in a 500 mL Schlenk flask
  2. washThe column was washed with an additional 100 mL of anhydrous acetonitrile
  3. additionSubsequent evacuation of the vessel containing the combined yellow eluents to a constant weight over 24 hours

Sources & evidence

ORD record
ord-ade1e23959714101aa1a67c47f848752
Source dataset
uspto-grants-2016_04
Patent number
US09309266B2

Reaction notes

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