Method for preparing metallocene compounds

A technology of metallocene compounds and compounds, applied in the direction of metallocenes, chemical instruments and methods, compounds of group 4/14 elements of the periodic table, etc., can solve the problems of final yield decline, time-consuming, unsuitable for large-scale production, etc.

Inactive Publication Date: 2000-06-07
MONTELL TECH CO BV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] Even in this case, two separate reaction steps are required, as well as a metallocene dihalide intermediate isolation step, which significantly reduces the final yield and makes the whole process more tedious and time-consuming
[0014] Therefore, prior art processes for the production of metallocene derivatives containing hydrocarbon sigma ligands are unsuitable for the feasible practical large-scale production of said derivatives as catalyst components for olefin polymers, and the need has been felt for a method of producing such derivatives in good yields. A simpler and more convenient practical method for the production of the above-mentioned metallocene derivatives

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0060] rac-CH 2 (3-tert-butyl-1-indenyl) 2 ZrMe 2 Synthesis

[0061] Compound rac-CH 2 (3- t Bu-1-Ind) 2 ZrMe 2 , adopt the method of the present invention, prepare according to the following reaction scheme:

[0062] The ligand bis-(3-tert-butyl-1-indenyl)methane was prepared by the base-catalyzed condensation of indene with formaldehyde as described in Examples 3(a) and (b) of European Patent Application No 97200933.6.

[0063] In a 250 ml Schlenk tube, 6.0 g of pure bis(3-tert-butyl-1-indenyl)methane [molecular weight (MW) 356, 15.8 mmol] was dissolved in 120 ml of Et 2 O, the solution was cooled to -20 °C. Add 45 ml of 1.6M MeLi in Et dropwise with continuous stirring 2 O solution (72 mmol) for 15 min. The resulting solution was warmed to room temperature and stirred for 5 hours. After about 1.5 hours, the lithium salt started to precipitate, eventually forming an orange suspension.

[0064] 4.0g ZrCl 4 (MW233.03, 17.0mmol) was suspended in 120ml pentane. B...

example 2

[0076] Synthesis of Ethylenebis(4,7-Dimethyl-1-indenyl)zirconium Dimethyl

[0077] Using a dark glassware, dissolve 8.4ml of 1.6M MeLi in Et 2 O solution (13.44mmol), at -70°C, added to 30ml Et 2 A solution of 1 g of 1,2-bis(4,7-dimethyl-indenyl)ethane (3.2 mmol) in O for about 10 min. The mixture was slowly warmed to room temperature and maintained under stirring for 3 hours. An increase in turbidity was observed, eventually forming a white suspension.

[0078] The suspension was cooled to -80°C, and 0.746 g of ZrCl in 30 ml of pentane, also cooled to -80°C, was added rapidly thereto. 4 (3.2 mmol) mixture. The temperature was slowly raised to room temperature over 1 night (about 16 hours) to finally obtain a dark brown solution. The reaction mixture was then dried under reduced pressure. The brown solid thus obtained was extracted with 40 ml of toluene, and the filtrate was evaporated to dryness under reduced pressure, thus obtaining 1.12 g (yield 80.7%) of a pale yello...

example 3

[0089] Synthesis of Ethylene Bis(1-Indenyl)Zirconium Dimethyl

[0090] Using a dark glassware, dissolve 8.4ml of 1.6M MeLi in Et 2 O solution (13.44mmol), at -70°C, added to 30ml Et 2 In a solution containing 0.82 g of bis(indenyl)ethane (3.2 mmol, G.C. purity 90%) in O for about 10 minutes. The resulting mixture was slowly warmed to room temperature and stirred for 3 hours. An increase in turbidity was observed, eventually forming a white suspension.

[0091] The white suspension was cooled to -80°C, and 0.746g of ZrCl in 30ml of pentane cooled to -80°C was added rapidly thereto. 4 (3.2 mmol) mixture. The temperature was slowly raised to room temperature over 1 night (about 16 hours) to finally obtain a dark brown solution. The reaction mixture was then dried under reduced pressure. The brown solid was extracted with 40 ml of toluene, and the filtrate was evaporated to dryness under reduced pressure, thus obtaining 0.67 g (61.6% yield) of a pale yellow solid. 1 H-NMR a...

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Abstract

A new process is disclosed, particularly simple, convenient and practical, for the direct synthesis of metallocenes of formula (I): (CP)(ZR1m)n(A)rMLpL'q wherein (ZR1m)n is a divalent group bridging Cp and A; Cp is a substituted or unsubstituted cyclopentadieryl group; A is -O-, -S-, -N(R2)-, wherein R2 is hydrogen, alkyl, cycloalkyl aryl, alkylaryl or arylalkyl, or A has the same meaning of Cp; M is a transition metal belonging to group 3, 4, 5, 6 or to the lanthanide or actinide groups; L is a monoanionic sigma ligand, such as alkyl, cycloalkyl, aryl, alkylaryl or arylalkyl, optionally containing Si or Ge; L' is halogen or -OR5, R5 being a hydrocarbon radical; m is 1 or 2; n is 0-4; r is 0 or 1; p is 1-3; q is 0-2. Said process comprises reacting the ligand (Y-Cp)(ZR1m)n(A-Y)r, wherein Y is a suitable leaving group, with at least 1 molar equivalent of ML's in the presence of at least (1+r+p) molar equivalents of LjB or LMgL', wherein B is an alkaline or alkaline-earth metal, s ranges from 3 to 6, and j is 1 or 2.

Description

field of invention [0001] The present invention relates to a novel method for the preparation of metallocene compounds which is particularly simple, convenient and practical; more precisely, it relates to a method for the direct synthesis of metallocenes in which the transition metal atom has at least one sigma ligand, said Ligands are selected from linear or branched, saturated or unsaturated C 1 ~C 20 Alkyl, C 3 ~C 20 Cycloalkyl, C 6 ~C 20 Aryl, C 7 ~C 20 Alkaryl and C 7 ~C 20 Aralkyl, optionally containing Si or Ge atoms. These metallocenes are used, for example, as catalyst components in olefin polymerization, oligomerization and hydrogenation reactions, in combination with aluminoxanes and / or compounds capable of forming alkyl metallocene cations. Background technique [0002] Homogeneous catalytic systems based on the combination of metallocenes and alkylaluminum compounds or alumoxanes are well known in the art and have been widely used in the polymerization...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/10C07F7/00C07F17/00C08F4/642C08F10/00
CPCY10S526/943C07F17/00C08F10/00C08F4/65927
Inventor L·雷斯科尼D·巴尔波尼G·普里尼
Owner MONTELL TECH CO BV
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