반응 #319291

반응 방정식

ferrocene

iron(III) chloride

ethanol

→

ferrocene

iron chloride

용매

ether

반응 조건

후처리

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

실험 절차

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.

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