Aluminium fluoride--water (1/3/3) → HCID 22044322, compound

HRID 2373862Notes

Reaction equation

HRID 2373862 reaction equation
O.O.O.[F-:4].[Al+3:5].[F-:6].[F-:7].O.O.O.[F-:11].[CH2:12]([N+:14]([CH2:18][CH3:19])([CH2:16][CH3:17])[CH3:15])[CH3:13]>>[F:4][Al-:5]([F:11])([F:7])[F:6].[CH2:12]([N+:14]([CH2:18][CH3:19])([CH2:16][CH3:17])[CH3:15])[CH3:13]

Participants

3

Reactant 2

HCID 22002992Aluminium fluoride--water (1/3/3)HCID 131727208HCID 131727208, compound

Product 1

HCID 22044322HCID 22044322, compoundYield 82.1%

Procedure

6.90 g (50.0 mmol) of aluminum fluoride trihydrate was weighed and placed in a round flask made of PFA, and air in the flask was evacuated and then replaced by argon gas. While feeding argon gas to the flask through its inlet, 100 ml of dehydrated acetonitrile was added and the flask was sealed followed by stirring for 30 minutes. Then, while feeding argon gas similarly, 9.46 g (50.0 mmol) of triethylmethylammonium fluoride trihydrate was added portion wise, and the resultant mixture was further stirred for about 3 hours. The unreacted solid was filtered off, and then the solvent was distilled off to obtain about 9 g of white crude crystal of triethylmethylammonium tetrafluoroaluminate. This was subjected to recrystallization from 10 g of isopropanol. The amount of the product was 5.50 g, and the yield was 50% based on the charged raw material. Identification was made by elemental analysis and NMR, and a melting point was measured by TG-DTA.

Workup

  1. customplaced in a round flask
  2. customwas evacuated
  3. additionwas added
  4. customthe flask was sealed
  5. filtrationThe unreacted solid was filtered off
  6. distillationthe solvent was distilled off

Sources & evidence

ORD record
ord-ca2e843a9a1646cc8c31678ed4911c13
Source dataset
uspto-grants-2008_12
Patent number
US07460357B2

Reaction notes

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