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Synthesis of metal complexes and uses thereof

a metal complex and metal complex technology, applied in the direction of organic compound/hydride/coordination complex catalyst, organic compound/compound/complex catalyst, group 3/13 element organic compound, etc., can solve the problem of large-scale implementation impracticality, and the alkali metal salt of carbonyl cobaltate utilized for synthesis is not commercially availabl

Inactive Publication Date: 2017-08-10
NOVOMER INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

The patent text describes a method for making catalysts with very low amounts of contamination from halide and alkali metal salts. The catalysts formed have a halide content of less than 2000 ppm and an alkali metal salt content of less than 2000 ppm. The technical effect of this invention is the production of highly pure catalysts with improved activity and selectivity for chemical reactions.

Problems solved by technology

Unfortunately, this procedure has features that make its implementation on large scale impractical.
Firstly, the alkali metal salt of the carbonyl cobaltate utilized for the synthesis is not commercially available and must be formed in a separate step (typically from dicobalt octacarbonyl) then isolated and purified prior to use.
Typically, this is done by recrystallizing the air sensitive catalyst which, while practicable at laboratory scale, is problematic at production volumes.

Method used

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  • Synthesis of metal complexes and uses thereof
  • Synthesis of metal complexes and uses thereof
  • Synthesis of metal complexes and uses thereof

Examples

Experimental program
Comparison scheme
Effect test

example 3

ntent of Aluminum Complexes

[0264]Using ICP-AES, the sodium content of the products of Examples 1 and 2 was measured and found to be below the detectable limit. In contrast, the sodium content of the same complexes prepared by salt metathesis were found to have sodium wt % in the range of 0.04 to 0.23 for 10 different preparations.

example 4

of Ketones

[0265]In an NMR spectrum of the reaction product resulting from treatment of (TPP)AlEt with 0.5 eq. of Co2(CO)8, 0.24 molar equiv. of pentanone (relative to the catalyst) was observed in the 1H NMR spectrum after the reaction. In addition, butane was detected in the volatiles from the filtrate and hexanes wash of the crystallized catalyst.

example 5

l Syntheses

[0266]Using the procedures described in Examples 1 and 2, the aluminum complexes [(OEP)Al(THF)2][Co(CO)4] and [(MeOTPP)Al(THF)2][Co(CO)4] can also be made by starting with the appropriate aluminum ligand (i.e., octaethylporphyrin or 5,10,15,20-tetrakis(4-methoxyphenyl)porphyrin).

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Abstract

The present disclosure provides novel methods of making aluminum complexes with utility for promoting epoxide carbonylation reactions. Methods include reacting neutral metal carbonyl compounds with alkylaluminum complexes.

Description

CROSS REFERENCE TO RELATED APPLICATIONS[0001]The present invention claims priority to U.S. provisional patent application No. 62 / 028,993, filed Jul. 25, 2014, the entire contents of which are hereby incorporated by reference.ACKNOWLEDGMENT OF GOVERNMENT SUPPORT[0002]This invention was made with Government support under Grant No. DE-EE0005766, awarded by the Department of Energy. The government has certain rights in the invention.BACKGROUND OF THE INVENTION[0003]Bimetallic complexes containing a cationic metal-centered Lewis acid in combination with an anionic metal carbonyl are highly active catalysts for the ring-expanding carbonylation of strained heterocycles, including epoxides, aziridines, oxetanes and lactones. In particular, such bimetallic catalysts comprising a cationic aluminum complex as a Lewis-acidic component and a carbonyl cobaltate anion are useful for the double carbonylation of epoxides to succinic anhydrides (Rowley et al., J. Am. Chem. Soc., 2007, 129, 4948-4960)...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): B01J31/18C07F5/06
CPCB01J31/183C07F5/069B01J2531/845B01J2531/025B01J2531/31B01J2231/321B01J31/1815B01J31/2243B01J2531/0205B01J2531/0252C07C45/86C07D487/22
Inventor LEE, HAN
Owner NOVOMER INC
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