IP Library › Granted Patent US 11,554,365
Granted Patent B2
US 11,554,365 · App. 17/677,102 · Granted Jan 17, 2023

Organoruthenium carbide complexes as precatalysts for olefin metathesis

Inventors: Rafał Gawin (Wroclaw, PL); Oleksandr Burtovyy (Akron, OH); Larry F Rhodes (Akron, OH)
Assignee: APEIRON SYNTHESIS S.A.
B01J31/2273B01J31/2278B01J31/24B01J31/2404C07C6/04C07D207/02C07D211/04C07D235/00C07F15/0046B01J2231/543B01J2531/821C07C6/02C07C6/06C07C2531/22
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Quick Facts
Patent No.
US 11,554,365
App. No.
17/677,102
Granted
Jan 17, 2023
Kind
B2
Abstract

Embodiments in accordance with the present invention encompass an organoruthenium compound of the formula (I) or formula (II): Wherein X, L, R 1 , R 2 , R 3 , R 4 , R 5 , Ar 1 and Ar 2 are as defined herein. Also disclosed herein are the use of organoruthenium compound of formula (I) or formula (II) as (pre)catalysts for the olefin metathesis reactions, as well as to the process for carrying out the olefin metathesis reaction.

Claims (58)

1. A compound of formula II:

wherein:

X is chlorine, bromine or iodine;

L is PR 3 , where R is independently selected from the group consisting of isopropyl, sec-butyl, tert-butyl, cyclohexyl, bicyclo(C 5 -C 10 )alkyl, phenyl, benzyl, isopropoxy, sec-butoxy, tert-butoxy, cyclohexyloxy, phenoxy and benzyloxy;

R 2 and R 3 are the same or different and each independently selected from the group consisting of hydrogen, methyl, ethyl, linear or branched (C 1 -C 6 )alkyl, (C 6 -C 10 )aryl, methoxy, ethoxy, linear or branched (C 1 -C 6 )alkoxy, (C 6 -C 10 )aryloxy, —NHCO(C 1 -C 6 )alkyl, —NHCO-perfluoro(C 1 -C 6 )alkyl, —SO 2 N((C 1 -C 6 )alkyl) 2 and —NO 2 ; or

R 2 and R 3 taken together with the carbon atom to which they are attached to form a (C 3 -C 7 )cycloalkyl ring;

R 4 and R 5 are the same or different and each independently selected from the group consisting of hydrogen, methyl, ethyl and linear or branched (C 1 -C 6 )alkyl;

Ar 2 is selected from the group consisting of substituted or unsubstituted phenyl, substituted or unsubstituted biphenyl and substituted or unsubstituted naphthyl;

wherein said substituents are selected from the group consisting of methyl, ethyl, iso-propyl, tert-butyl and phenyl.

2. The compound according to claim 1 , wherein:

X is chlorine or iodine;

each R 2 , R 3 , R 4 and R 5 is independently selected from the group consisting of methyl, ethyl, n-propyl, iso-propyl, n-butyl, iso-butyl, tert-butyl and phenyl;

Ar 2 is substituted phenyl; and

L is PR 3 , where each R is independently selected from the group consisting of isopropyl, sec-butyl, tert-butyl, cyclohexyl and phenyl.

3. The compound according to claim 1 , wherein:

X is chlorine;

R 2 and R 3 taken together with the carbon atom to which they are attached to form a cyclopentyl, cyclohexyl or cycloheptyl ring;

each R 4 and R 5 is independently selected from the group consisting of hydrogen, methyl, ethyl and iso-propyl;

Ar 2 is selected from the group consisting of phenyl, 2-methylphenyl,

2,4-dimethylphenyl, 2,6-dimethylphenyl, 2,4,6-trimethylphenyl, 2-ethylphenyl,

2,4-diethylphenyl, 2,6-diethylphenyl, 2,4,6-triethylphenyl, 2-isopropylphenyl and 2,6-diisopropylphenyl; and

L is tri(isopropyl)phosphine or tricyclohexylphosphine.

4. The compound according to claim 1 , wherein:

X is chlorine;

each R 2 , R 3 , R 4 and R 5 independently is methyl or ethyl;

Ar 2 is selected from the group consisting of phenyl, 2,4-dimethylphenyl,

2,6-dimethylphenyl, 2,4,6-trimethylphenyl, 2,4-diethylphenyl, 2,6-diethylphenyl,

2,4,6-triethylphenyl, 2-isopropylphenyl and 2,6-diisopropylphenyl; and

L is tricyclohexylphosphine.

5. The compound according to claim 1 , wherein:

X is iodine;

each R 2 , R 3 , R 4 and R 5 independently is methyl or ethyl;

Ar 2 is selected from the group consisting of 2,6-dimethylphenyl,

2,4,6-trimethylphenyl, 2,6-diethylphenyl, 2,4,6-triethylphenyl and 2,6-diisopropylphenyl; and

L is tricyclohexylphosphine.

6. The compound according to claim 1 , which is:

1-(2,6-diethylphenyl)-3,3,5,5-tetramethylpyrrolidin-2-ylidene-triisopropylphosphine ruthenium carbide dichloride.

7. The compound according to claim 1 , which is:

1-(2,6-diisopropylphenyl)-3,3,5,5-tetramethylpyrrolidin-2-ylidene-triisopropylphosphine ruthenium carbide dichloride.

8. The compound according to claim 1 , which is:

1-(2,6-diethylphenyl)-3,3,5,5-tetramethylpyrrolidin-2-ylidene-triisopropylphosphine ruthenium carbide diiodide.

9. The compound according to claim 1 , which is:

1-(2,6-diethylphenyl)-3,3,5,5-tetramethylpyrrolidin-2-ylidene-triisopropylphosphine ruthenium carbide diiodide.

10. The compound according to claim 1 , which is:

1-(2,6-diisopropylphenyl)-3,3-dimethyl-2λ 2 -azaspiro[4.5]decylidene-triisopropylphosphine ruthenium carbide dichloride.

11. The compound according to claim 1 , which is:

1-(2,6-diisopropylphenyl)-3,3-dimethyl-2λ 2 -azaspiro[4.5]decylidene-triisopropylphosphine ruthenium carbide diiodide.

12. The compound according to claim 1 , which is:

1-(2,6-diethylphenyl)-3,5,5-trimethyl-3-phenylpyrrolidin-2-ylidene-triisopropylphosphine ruthenium carbide dichloride.

13. The compound according to claim 1 , which is:

1-(2,6-diethylphenyl)-3,5,5-trimethyl-3-phenylpyrrolidin-2-ylidene-triisopropylphosphine ruthenium carbide diiodide.

14. A process for carrying out a metathesis reaction of olefins, comprising contacting at least one olefin with the compound of claim 1 as a precatalyst.

15. The process according to claim 14 , wherein the metathesis reaction is carried out in an organic solvent.

16. The process according to claim 15 , wherein the organic solvent is selected from the group consisting of dichloromethane, dichloroethane, toluene, ethyl acetate and a mixture in any combination thereof.

17. The process according to claim 14 , wherein the metathesis reaction is carried out in the presence of a chemical activator.

18. The process according to claim 17 , wherein the chemical activator is a Bronsted or Lewis acid or a halo-derivative of alkane or silane.

19. The process according to claim 14 , wherein the metathesis reaction is carried out in the presence of a photoacid generator.

20. The process according to claim 14 , wherein the metathesis reaction is carried out in the presence of a thermal acid generator.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 21, 2024
From: PROMERUS, LLC
To: SUMITOMO BAKELITE CO., LTD.
Reel/Frame 069364/0733 →
Continuity (3)
Division 17024778 · Sep 18, 2020
Provisional Application 62901860 · Sep 18, 2019
Related Publication 20220176362A1 · Jun 9, 2022
Cited By (1)
US 12,251,688