Tetrafluoroboric acid → Triethylmethylphosphonium tetrafluoroborate
Reaction equation
[OH-].[CH2:2]([P+:4]([CH2:8][CH3:9])([CH2:6][CH3:7])[CH3:5])[CH3:3].[F:10][B-:11]([F:14])([F:13])[F:12].[H+]>>[F:10][B-:11]([F:14])([F:13])[F:12].[CH2:2]([P+:4]([CH2:8][CH3:9])([CH2:6][CH3:7])[CH3:5])[CH3:3]Participants
3
Conditions
- Temperature
- 28 °C
Procedure
To 1,581.5 g (0.859 mole) of 8.92 weight percent triethylmethylphosphonium hydroxide aqueous solution prepared as above, 180.45 g (0.863 mole) of 42% fluoroboric acid was added. The resulting transparent and colorless solution was stirred at a room temperature of 28° C. for 1 hour. The solution was concentrated using a rotary evaporator under a reduced pressure to obtain 406.2 g of slurry. The slurry was cooled at 15° C. for about 2 hours, and was filtered to recover white crystals (189.63 g). The crystals were dried at 110° C. overnight to yield 168.40 g of triethylmethylphosphonium tetrafluoroborate. The Br ion concentration determined by silver nitrate titration was 4 ppm.
Workup
- additionwas added
- concentrationThe solution was concentrated
- customa rotary evaporator under a reduced pressure
- customto obtain 406.2 g of slurry
- temperatureThe slurry was cooled at 15° C. for about 2 hours
- filtrationwas filtered
- customto recover white crystals (189.63 g)
- customThe crystals were dried at 110° C. overnight
Sources & evidence
- ORD record
- ord-2a73703c41ef44949d8fd63e7a771a1e
- Source dataset
- uspto-grants-2003_11
- Patent number
- US06649728B2
Reaction notes
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