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Method for preparing semi-cyclopentadienyl vanadium

A technology of compounds and substituents, applied in the field of preparation of semi-vanacene compounds, can solve the problems of inability to produce semi-vanacene compounds, high yield, impractical semi-vanacene compounds, etc.

Inactive Publication Date: 2003-05-28
UBE IND LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, when not using purified (C 5 h 5 ) 2 VCl 2 When used as a raw material, high-purity (C 5 h 5 ) VCl 3
[0010] As mentioned above, prior art methods for preparing hemivanacene compounds are not practical because the starting compounds may decompose and the hemivanacene compounds cannot be produced in sufficiently high yields

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0105] (a) Preparation of Vanacene Compounds

[0106] Vanadium tetrachloride (2.3 kg) was dissolved in 20 liters of tetrahydrofuran at -10°C. The solution was kept at -10 °C while adding 27 liters (C 5 h 5 ) Na in tetrahydrofuran (concentration is 0.88 mol / liter). With (C 5 h 5 ) Na was added dropwise, and a solid was gradually precipitated out. The resulting suspension was stirred while warming to 50°C over 16 hours. While maintaining the temperature at 50° C., tetrahydrofuran was evaporated under reduced pressure and the residue was vacuum-dried for 3 hours to obtain 5.1 kg of a light gray-green vanacene compound solid. Analysis showed that the solid contained 2.27 mol / kg of (C 5 h 5 ) 2 VCl 2 .

[0107] (b) Chlorination

[0108] 300 g of the vanacene compound obtained was suspended in 2 liters of chloroform, and the suspension was heated to 50°C. Chlorine gas was introduced (gas flow rate: 3.6 liters / hour) while continuously adding 7.5 ml of water over 9 hours ...

Embodiment 2

[0109] (a) Preparation of Vanacene Compounds

[0110] Prepare vanacene compound in the same way as Example 1 (a), (C 5 h 5 ) 2 VCl 2 .

[0111] (b) Chlorination

[0112] 150 g of the obtained vanacene compound was suspended in 1 liter of chloroform, and the suspension was heated to 50°C. Chlorination was carried out by supplying chlorine gas (gas flow of 2 liters / hour) and oxygen gas (gas flow of 0.6 liters / hour) continuously for 8 hours. After chlorination, carry out the refining step identical with embodiment 1 (b), obtain 40g (C 5 h 5 )VOCl 2 (Yield 58%). Example 13

Embodiment 13

[0113] Except using hexane as the solvent of chlorination reaction, carry out and embodiment 1 identical steps, obtain (C 5 h 5 )VOCl 2 . Example 4

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PUM

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Abstract

A process for preparing a half-vanadocene compound, the process comprising reacting chlorine gas with a vanadocene compound represented by the formula (1) Cp2VX2 wherein Cp represents cyclopentadienyl, substituted cyclopentadienyl, indenyl, substituted indenyl, fluorenyl, substituted fluorenyl, benzoindenyl, substituted benzoindenyl, azulenyl or substituted azulenyl, and the two Cp groups may be the same or different, X represents fluorine, chlorine, bromine or iodine and the two X atoms may be the same or different.

Description

technical field [0001] The present invention relates to a preparation method of a hemivanacene compound, more particularly to a method for preparing a hemivanacene compound with a high yield using a chemically stable vanadium compound as a starting material. Background technique [0002] Semivanacene compounds, typically vanadium complexes of cyclopentadiene, are widely used as catalysts for the polymerization of olefins or dienes. Semivanacene compounds show high activity as catalysts for the polymerization of butadiene, and it is an indispensable and important catalyst in organic synthesis. [0003] Examples of semivanacene compounds include (C 5 h 5 )VOCl 2 , (C 5 h 5 ) VCl 3 Wait. A number of methods are known for the preparation of such semivanacene compounds. [0004] According to reports, through (C 5 h 5 )V(CO) 4 React with a mixed gas of oxygen and chlorine to prepare (C 5 h 5 )VOCl 2 (J. Organomet. Chem., No. 319, page C21 (1987)). It is also reporte...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/00C07F17/00C08F4/44
CPCY10S526/943C07F17/00
Inventor 小原忠直久保朋也
Owner UBE IND LTD
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