((Dimethylamino)methylene)dimethylammonium methyl sulphate → 1066-47-3
Reaction equation
COS([O-])(=O)=O.[CH3:7][N:8]([CH3:13])[CH:9]=[N+:10]([CH3:12])[CH3:11].[F:14][P-:15]([F:20])([F:19])([F:18])([F:17])[F:16].[NH4+]>O>[F:14][P-:15]([F:20])([F:19])([F:18])([F:17])[F:16].[CH3:11][N:10]([CH3:12])[CH:9]=[N+:8]([CH3:13])[CH3:7]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 0 °C
Procedure
N,N,N′,N′-tetramethylformamidinium methylsulfate (3 g) is added to water (25 ml) and the resulting mixture is cooled to 0° C. This mixture is then added to a cooled solution of ammonium hexafluorophosphate (4.6 g) in water (25 ml). The so formed precipitate is then collected by filtration. The precipitate is washed with cold water (2×10 ml) and then with diethyl ether (10 ml). Drying in vacuo gives N,N,N′,N′-tetramethylformamidinium hexafluorophosphate (18, R6=Me, R7=Me) as a white solid. 1H NMR (DMSO-d6), 7.90 (1H), 3.26 (6H), 3.14 (6H).
Workup
- customThe so formed precipitate
- filtrationis then collected by filtration
- washThe precipitate is washed with cold water (2×10 ml)
- customDrying in vacuo
Sources & evidence
- ORD record
- ord-94b82acf8cdc45b0a93772c8149ccb38
- Source dataset
- uspto-grants-2016_01
- Patent number
- US09227934B2
Reaction notes
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