Ethanol → Bis(eta-cyclopentadienyl) iron

HRID 232109

反応式

HRID 232109 の反応式
[CH-:1]1[CH:5]=[CH:4][CH:3]=[CH:2]1.[CH-:6]1[CH:10]=[CH:9][CH:8]=[CH:7]1.[Fe+2].[Fe:12](Cl)([Cl:14])[Cl:13].C(O)C>CCOCC>[CH-:1]1[CH:5]=[CH:4][CH:3]=[CH:2]1.[CH-:6]1[CH:10]=[CH:9][CH:8]=[CH:7]1.[Fe+2:12].[Fe:12]([Cl:14])[Cl:13]

参加物

6

反応物 3

HCID 702EthanolHCID 7611Bis(eta-cyclopentadienyl) ironHCID 24380Iron chloride (FeCl3)

生成物 2

HCID 7611Bis(eta-cyclopentadienyl) ironHCID 24458Ferrous Chloride

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-addad72e6a94407f99e85273bd235b03
出典データセット
uspto-grants-1989_07
特許番号
US04851430

関連ノート

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