関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Bis(eta-cyclopentadienyl) iron | HCID 7611 | — |
| 反応物 | Iron chloride (FeCl3) | HCID 24380 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | Bis(eta-cyclopentadienyl) iron | HCID 7611 | — |
| 生成物 | Ferrous Chloride | HCID 24458 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04851430 |
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| 出典データセット | uspto-grants-1989_07 |
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| ORD ID | ord-addad72e6a94407f99e85273bd235b03 |
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| 出典メモ | uspto-grants-1989_07 |
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