Reaktion #319291

ord-addad72e6a94407f99e85273bd235b03

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeobtained
  2. 2
    Sonstigecan be recrystallized either from freshly distilled thionyl chloride or from 0.15-0.25M aqueous-methanolic (2:98) hydrogen chloride
  3. 3
    Sonstigebeing obtained in the form of blue-black crystal flakes
  4. 4
    SonstigeThe recrystallization from the acid medium

Vorschrift

Impure ferricenium tetrachloroferrate is prepared from ferrocene (2 mmol) and anhydrous iron(III) chloride (4 mmol) in ether, with recrystallization from absolute ethanol, by the process of Nesmeyanov et al. The product obtained, the infrared spectrum of which shows that it is a product contaminated with diferricenium μ-oxo-bis(trichloroferrate), can be recrystallized either from freshly distilled thionyl chloride or from 0.15-0.25M aqueous-methanolic (2:98) hydrogen chloride, a ferricenium tetrachloroferrate which is pure according to spectroscopy (disappearance of the maxima at 365 and 316 cm-1) and elemental analysis being obtained in the form of blue-black crystal flakes. Found: C, 31.22; H, 2.71; Cl, 36.80. Calculated for C10H10Cl4Fe2 : C, 31.30; H, 2.63; Cl, 36.96. The recrystallization from the acid medium can also be carried out directly with the crude product obtained from ferrocene and iron chloride, by-avoiding the recrystallization from absolute ethanol.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04851430uspto-grants-1989_07