Hydrofluoric Acid → Hydrofluoric Acid
Reaction equation
[Cl-].[CH2:2]([O:4][CH2:5][N+:6]1([CH3:11])[CH2:10][CH2:9][CH2:8][CH2:7]1)[CH3:3].[FH:12]>>[FH:12].[F-:12].[CH2:2]([O:4][CH2:5][N+:6]1([CH3:11])[CH2:10][CH2:9][CH2:8][CH2:7]1)[CH3:3]Participants
Conditions
- Temperature
- 60 °C
Procedure
N-ethoxymethyl-N-methylpyrrolidinium chloride (60.90 g) was mixed with a solution of hydrofluoric acid. N2 was bubbled through the mixture with heating at 60° C. to remove hydrogen chloride and an excess of hydrofluoric acid and obtain 62.10 g of N-ethoxymethyl-N-methylpyrrolidinium fluoride. In 1000 g of 50% aqueous solution of hydrofluoric acid was dissolved 156 g of aluminum hydroxide at room temperature and the mixture was filtered. The filtrate was cooled to obtain 442.76 g of aluminum fluoride nonahydrates. To 46.70 g of the above N-ethoxymethyl-N-methylpyrrolidinium fluoride was added 53.40 g of aluminum fluoride nonahydrates at 50° C. with stirring. N2 was bubbled through the mixture with heating at 130° C. to remove hydrofluoric acid and obtain 46.80 g of the desired product (brown liquid). The product was checked for 1H-NMR and electrical conductivity as in Example 1.
Workup
- customN2 was bubbled through the mixture
- customto remove hydrogen chloride
Sources & evidence
- ORD record
- ord-ae43e13c9e984bdfb29db169df549904
- Source dataset
- uspto-grants-2011_01
- Patent number
- US07875732B2
Reaction notes
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