Method for producing Tebbe complex

Patent metadata

Field	Value
Publication number	US-10017534-B2
Application number	US-201515514977-A
Country	US
Kind code	B2
Filing date	Sep 18, 2015
Priority date	Sep 29, 2014
Publication date	Jul 10, 2018
Grant date	Jul 10, 2018

Abstract

The present invention relates to a method for producing a Tebbe complex having high purity and high activity and having excellent storage stability in a high yield, the method including allowing bis(cyclopentadienyl)titanium dichloride and trimethylaluminum to react with each other in the presence of a solvent such that a solubility of the Tebbe complex in 1 g of the solvent at 25° C. is 0.5 mmol/g or less.

First claim

The invention claimed is:

1. A method for producing a Tebbe complex, the method comprising
reacting bis(cyclopentadienyl)titanium dichloride with trimethylaluminum in the presence of a solvent such that a solubility of the Tebbe complex in 1 g of the solvent at 25° C. is 0.5 mmol/g or less, thereby obtaining a reaction liquid,
wherein a charged amount of the bis(cyclopentadienyl)titanium dichloride is from 0.1 to 2.5 mmol/g in terms of a titanium atom concentration relative to the solvent.

2. The method according to claim 1 , wherein the solvent is an aliphatic hydrocarbon having 3 to 20 carbon atoms.

3. The method according to claim 2 , wherein the aliphatic hydrocarbon having 3 to 20 carbon atoms is at least one selected from the group consisting of a straight-chain aliphatic hydrocarbon having 3 to 20 carbon atoms and a branched aliphatic hydrocarbon having 3 to 20 carbon atoms.

4. The method according to claim 1 , wherein a charged amount of the trimethylaluminum is one to twenty molecules relative to one molecule of the bis(cyclopentadienyl)titanium dichloride.

5. The method for producing a Tebbe complex according to claim 1 , wherein said reacting is performed at a temperature of from 0 to 125° C.

6. The method for producing a Tebbe complex according to claim 1 , wherein said reacting is performed for a time of from 1 to 200 hours.

7. The method for producing a Tebbe complex according to claim 1 , further comprising
recovering the Tebbe complex in a solid state as deposited from the reaction liquid by filtration or decantation.

8. The method according to claim 1 , further comprising
concentrating the reaction liquid at a concentration temperature of 10 to 125° C. under a pressure of 0.001 to 0.100 MPaG.

9. The method according to claim 1 , further comprising
subjecting the reaction liquid to a crystallization operation at a crystallization temperature of −10 to 20° C. for a time of 30 minutes or more.

10. The method according to claim 1 , further comprising
washing the Tebbe complex with a hydrocarbon solvent,
wherein the hydrocarbon solvent has a dielectric constant of 1.0 to 5.0.

11. The method according to claim 1 , further comprising
storing the Tebbe complex in the presence of a solvent such that a solubility of the Tebbe complex in 1 g of the solvent at 25° C. is more than 0.5 mmol/g.

Assignees

• Kuraray Co

Inventors

• Hatae Shinji
• Sunaga Syuichi
• Tsuji Tomoaki

Classifications

• B01J2231/645

  of C=C or C-C triple bonds · CPC title

• B01J31/2295

  Cyclic compounds, e.g. cyclopentadienyls · CPC title

• B01J2531/0208

  Bimetallic complexes, i.e. comprising one or more units of two metals, with metal-metal bonds but no all-metal (M)n rings, e.g. Cr2(OAc)4 · CPC title

• C07F5/062

  Al linked exclusively to C · CPC title

• C07F17/00 Primary

  Metallocenes · CPC title