Perchloric Acid → Hexafluorophosphate

HRID 374956Notes

Reaction equation

HRID 374956 reaction equation
[Cl:1]([OH:5])(=[O:4])(=[O:3])=[O:2].[F:6][P-:7]([F:12])([F:11])([F:10])([F:9])[F:8].[H+]>CCOCC>[Cl:1]([O-:5])(=[O:4])(=[O:3])=[O:2].[F:6][P-:7]([F:12])([F:11])([F:10])([F:9])[F:8]

Participants

5

Reactant 2

HCID 24247Perchloric AcidHCID 16211447Hexafluorophosphoric acid

Product 2

HCID 9886HexafluorophosphateHCID 123351Perchlorate

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent

Procedure

A mixture of one of these anthranils (1 part) and a tert-alkanol (1.1 to 1.2 parts) is warmed to effect solution, then is cooled in an ice-water bath while 70% perchloric acid or 60% hexafluorophosphoric acid (2 parts) is added at a rate which maintained the internal reaction temperature ≤35° C. After addition, the reaction mixture is stirred with ice-water cooling while the precipitate formed over about 30 minutes. This is slurried in ether and the salts are collected by filtration, washed with dry ether, and dried under vacuum to give the N-tert-alkyl anthranilium perchlorate or hexafluorophosphate salt as pale yellow solids in high yields.

Workup

  1. additionis added at a rate which
  2. temperaturemaintained the internal reaction temperature ≤35° C
  3. additionAfter addition
  4. customformed over about 30 minutes
  5. filtrationthe salts are collected by filtration
  6. washwashed with dry ether
  7. customdried under vacuum

Sources & evidence

ORD record
ord-f8537ef70a554f9b9391f86bcff8e0ea
Source dataset
uspto-grants-1996_01
Patent number
US05482974

Reaction notes

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