Tungsten → Tungsten Bis-triflimide

HRID 890860Notes

Reaction equation

HRID 890860 reaction equation
[W:1].[NH:2]([S:10]([C:13]([F:16])([F:15])[F:14])(=[O:12])=[O:11])[S:3]([C:6]([F:9])([F:8])[F:7])(=[O:5])=[O:4]>O>[NH:2]([S:3]([C:6]([F:9])([F:7])[F:8])(=[O:5])=[O:4])[S:10]([C:13]([F:16])([F:15])[F:14])(=[O:12])=[O:11].[NH:2]([S:3]([C:6]([F:9])([F:7])[F:8])(=[O:5])=[O:4])[S:10]([C:13]([F:16])([F:15])[F:14])(=[O:12])=[O:11].[W:1]

Participants

4

Reactant 2

HCID 23964TungstenHCID 157857Bis(trifluoromethane)sulfonimide

Product 1

HCID 131725283Tungsten Bis-triflimide

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
150 °C

Procedure

Tungsten metal (1.0 g, 99% purity) filings were suspended in water (20 mL) and hydrogen bis-triflimide (HNTf2) (5 g) was added. This mixture was heated under reflux for 144 hours. The resultant slurry was cooled, filtered and concentrated on a rotary evaporator to give a colourless solution that crystalised on standing. The crystals were heated at 150° C. at 1 mmHg to remove the residual water and hydrogen bis-triflimide. The precise structure of the catalyst is not known, but it was found to be the best of all isolated metal bis-triflimide catalysts tested in the reaction of benzoyl chloride with toluene.

Workup

  1. temperatureThis mixture was heated
  2. temperatureunder reflux for 144 hours
  3. temperatureThe resultant slurry was cooled
  4. filtrationfiltered
  5. concentrationconcentrated on a rotary evaporator
  6. customto give a colourless solution that
  7. customcrystalised
  8. customto remove the residual water and hydrogen bis-triflimide
  9. customtested in the reaction of benzoyl chloride with toluene

Sources & evidence

ORD record
ord-d7edf756bb7e4606a026aa316330c8fc
Source dataset
uspto-grants-2006_02
Patent number
US06998497B2

Reaction notes

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