Sulfate Ion → Bis(pentafluorophenyl)borinic acid

HRID 2415511

Reaktionsgleichung

Reaktionsgleichung von HRID 2415511
S([O-])([O-])(=O)=O.S([O-])([O-])(=O)=O.[Al+3].S([O-])([O-])(=O)=O.S([O-])([O-])(=O)=[O:18].[Al+3].[F:23][C:24]1[C:29]([B:30](C2C(F)=C(F)C(F)=C(F)C=2F)[C:31]2[C:36]([F:37])=[C:35]([F:38])[C:34]([F:39])=[C:33]([F:40])[C:32]=2[F:41])=[C:28]([F:53])[C:27]([F:54])=[C:26]([F:55])[C:25]=1[F:56]>C1(C)C=CC=CC=1>[F:23][C:24]1[C:29]([B:30]([C:31]2[C:36]([F:37])=[C:35]([F:38])[C:34]([F:39])=[C:33]([F:40])[C:32]=2[F:41])[OH:18])=[C:28]([F:53])[C:27]([F:54])=[C:26]([F:55])[C:25]=1[F:56]

Komponenten

5

Edukt 3

HCID 1117Sulfate Ion2×HCID 24850Aluminum SulfateHCID 582056Tris(pentafluorophenyl)borane

Produkt 1

HCID 9841889Bis(pentafluorophenyl)borinic acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

Moreover, that patent also discloses a method in which alminium sulfate 18 hydrate is used instead of water. Specifically, aluminium sulfate 18 hydrate is added to a toluene solution of tris (pentafluorophenyl) borane. After the solution is refluxed, insoluble alminium sulfate is separated from the reaction mixture. A solvent of a filtrate is removed in vacuo. Toluene is added to the thus obtained residue. After stirring, the insoluble matter passes through a G4 sintered-glass so as to be separated. The solvent of the filtrate is again removed in vacuo. Heptane is added to the residue. The solution is stirred and filtered so that a cake is obtained. Finally, the thus obtained cake is washed with heptane, and dried in vacuo so as to isolate bis (pentafluorophenyl) borinic acid. However, this method has such a problem that it is necessary to remove the by-product alminium sulfate and its process is so complicated.

Aufarbeitung

  1. customis separated from the reaction mixture
  2. customA solvent of a filtrate is removed in vacuo
  3. additionToluene is added to the thus obtained residue
  4. customto be separated
  5. customThe solvent of the filtrate is again removed in vacuo
  6. additionHeptane is added to the residue
  7. stirringThe solution is stirred
  8. filtrationfiltered so that a cake
  9. customis obtained
  10. washFinally, the thus obtained cake is washed with heptane
  11. customdried in vacuo so as

Quellen und Nachweise

ORD-Eintrag
ord-03415fdd158844aebd70c8ce41bb8f1a
Quelldatensatz
uspto-grants-2004_11
Patentnummer
US06818785B2

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