HRID232109

反应详情

EQUATION

反应方程式

HRID 232109 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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.

WORKUP

后处理

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