Chromium → Chromium(III) Bis-triflimide

HRID 890859Notes

Reaction equation

HRID 890859 reaction equation
[Cr: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].[Cr+3:1]

Participants

4

Reactant 2

HCID 23976ChromiumHCID 157857Bis(trifluoromethane)sulfonimide

Product 1

HCID 131725282Chromium(III) Bis-triflimide

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
150 °C

Procedure

Chromium metal (1.0 g, 99.95% purity) pieces 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 mixture was cooled, filtered and concentrated on a rotary evaporator to give a green solid. The solid were heated at 150° C. at 1 mmHg to remove the residual water and hydrogen bis-triflimide. The solid was thought to contain an oxo chromium bis-triflimide species CrO(NTf2) from the mass of HNTf2 produced in drying process. The unpurified chromium(III) bis-triflimide was found to display catalytic activity in Friedel-Crafts reactions, and was similar in activity to Zn(NTf2)2.

Workup

  1. temperatureThis mixture was heated
  2. temperatureunder reflux for 144 hours
  3. filtrationfiltered
  4. concentrationconcentrated on a rotary evaporator
  5. customto give a green solid
  6. customto remove the residual water and hydrogen bis-triflimide
  7. customproduced
  8. customin drying process

Sources & evidence

ORD record
ord-49b00927b3634fba9742ff99c9e7bec3
Source dataset
uspto-grants-2006_02
Patent number
US06998497B2

Reaction notes

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