Hydrofluoric Acid → Hydrofluoric Acid

HRID 254895Notes

Reaction equation

HRID 254895 reaction equation
[Cl-].[CH3:2][O:3][CH2:4][N+:5]1([CH3:10])[CH2:9][CH2:8][CH2:7][CH2:6]1.[FH:11]>>[FH:11].[F-:11].[CH3:2][O:3][CH2:4][N+:5]1([CH3:10])[CH2:9][CH2:8][CH2:7][CH2:6]1

Participants

4

Conditions

Temperature
60 °C

Procedure

N-methoxymethyl-N-methylpyrrolidinium chloride (50.0 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 59.52 g of N-methoxymethyl-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 30.4 g of the above N-methoxymethyl-N-methylpyrrolidinium fluoride was added 36.4 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 29.4 g of the desired product (brown liquid). The product was checked for 1H-NMR, electrical conductivity and voltage resistance as in Example 1.

Workup

  1. customN2 was bubbled through the mixture
  2. customto remove hydrogen chloride

Sources & evidence

ORD record
ord-a15ab90e21cf4e9cabb7dfb20594d3cf
Source dataset
uspto-grants-2011_01
Patent number
US07875732B2

Reaction notes

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