IP Library Granted Patent US 8,846,939
Granted Patent B2
US 8,846,939 · App. 13/494,708 · Granted Sep 30, 2014

Imidazolidine-based metal carbene metathesis catalysts

Inventors: Robert H. Grubbs (South Pasadena, CA); Matthias Scholl (Arcadia, CA)
Assignee: California Institute of Technology
C07F15/0046
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Quick Facts
Patent No.
US 8,846,939
App. No.
13/494,708
Granted
Sep 30, 2014
Kind
B2
Abstract

The present invention relates to novel metathesis catalysts with an imidazolidine-based ligand and to methods for making and using the same. The inventive catalysts are wherein: M is ruthenium or osmium; X and X 1 are each independently an anionic ligand; L is a neutral electron donor ligand; and, R, R 1 R 6 , R 7 , R 8 , and R 9 are each independently hydrogen or a substituent selected for the group consisting of C 1 C 20 alkyl, C 2 -C 20 alkenyl, C 2 -C 20 alkynyl, aryl, C 1 -C 20 alkoxycarbonyl, C 1 -C 20 alkyithiol, aryl thiol, C 1 -C 20 alkylsulfortyl and C 1 -C 20 alkylsulfinyl, the substituent optionally substituted with one or more moieties selected from the group consisting of C 1 -C 20 alkyl, C 1 -C 10 alkoxy, aryl, and a functional group. The inclusion of an imidazolidine ligand to the previously described ruthenium or osmium catalysts has been found to dramatically improve the properties of these complexes.

Claims (119)

1. A composition of matter comprising a compound having the formula:

where:

M is Ru or Os;

X and X 1 are each independently an anionic ligand;

P is phosphorus;

R g , R h and R i are each independently:

(1) a C 1-10 alkyl group,

(2) a C 3-10 cycloalkyl group or

(3) a C 5-20 aryl group;

R, R 6 , R 7 , R 8 , and R 9 are each independently:

(1) hydrogen,

(2) a C 1-10 alkyl group,

(3) a C 2-20 alkenyl group,

(4) a C 2-20 alkynyl group,

(5) an aryl group,

(6) a C 1-20 carboxylate group,

(7) a C 1-20 alkoxy group,

(8) a C 2-20 alkenyloxy group,

(9) a C 2-20 alkenyloxy group,

(10) an aryloxy group,

(11) a C 2-20 alkoxycarbonyl group,

(12) a C 1-20 alkylthiol group,

(13) a C 1-20 alkylsulfonyl group,

(14) a C 1-20 alkylsulfinyl group,

where each of R, R 6 , R 7 , R 8 , and R 9 is optionally substituted with

(a) halogen,

(b) a C 1-10 alkyl group,

(c) a C 1-10 alkoxy group,

(d) an aryl group

(e) a hydroxyl group,

(f) a thiol group,

(g) a thioester group,

(h) a ketone group,

(i) an aldehyde group,

(j) an ester group,

(k) an ether group,

(l) an amino group,

(m) an amido group,

(n) an imino group,

(o) a nitro group,

(p) a carboxylic acid group,

(q) a disulfide group,

(r) a carbonate group,

(s) an isocyanate group,

(t) a carbodiimide group,

(u) a carboalkoxy group, or

(v) a carbamate group.

2. An olefin metathesis catalyst wherein the metathesis catalyst has the following structure:

wherein,

M is ruthenium or osmium;

X and X 1 are each independently an anionic ligand;

L 1 is an imidazolidine ligand;

L is a neutral electron donor ligand; and

R and R 1 are each independently hydrogen, C 1-10 alkyl, C 2-20 alkenyl, C 2-20 alkynyl, aryl, C 1-20 carboxylate, C 1-20 alkoxy, C 2-20 alkenyloxy, C 2-20 alkynyloxy, aryloxy, C 2-20 alkoxycarbonyl, C 1-20 alkylthiol, aryl thiol, C 1-20 alkylsulfonyl, and C 1-20 alkylsulfinyl, and wherein each of R and R 1 is optionally substituted with halogen, C 1-10 alkyl, C 1-10 alkoxy, aryl, hydroxyl, thiol, thioether, ketone, aldehyde, ester, ether, amino, amido, imino, nitro, carboxylic acid, disulfide, carbonate, isocyanate, carbodiimide, carboalkoxy, or carbamate; and

wherein at least one of L, L 1 , R, R 1 , X, and X 1 may be linked with at least one of L, L 1 , R, R 1 , X, and X 1 to form a bonded ligand array or a bidentate ligand.

3. The metathesis catalyst of claim 2 , wherein the imidazolidine ligand has the following structure:

wherein,

R 6 , R 7 , R 8 , and R 9 are each independently hydrogen, C 1-10 alkyl, C 2-20 alkenyl, C 2-20 alkynyl, aryl, C 1-20 carboxylate, C 1-20 alkoxy, C 2-20 alkenyloxy, C 2-20 alkynyloxy, aryloxy, C 2-20 alkoxycarbonyl, C 1-20 alkylthiol, aryl thiol, C 1-20 alkylsulfonyl, and C 1-20 alkylsulfinyl, and wherein each of R 6 , R 7 , R 8 , and R 9 is optionally substituted with halogen, C 1-10 alkyl, C 1-10 alkoxy, aryl, hydroxyl, thiol, thioether, ketone, aldehyde, ester, ether, amino, amido, imino, nitro, carboxylic acid, disulfide, carbonate, isocyanate, carbodiimide, carboalkoxy, or carbamate.

4. The metathesis catalyst of claim 2 , wherein at least one of L, L 1 , R, R 1 , X, and X 1 is linked with at least one of L, L 1 , R, R 1 , X, and X 1 to form a bonded ligand array.

5. The metathesis catalyst of claim 2 , wherein L is bonded together with one of X and X 1 to form a bidentate ligand.

6. The metathesis catalyst of claim 2 , wherein L is bonded together with one of R and R 1 to form a bidentate ligand.

7. The metathesis catalyst of claim 2 , wherein R and R 1 are bonded together.

8. The metathesis catalyst of claim 2 , wherein the metathesis catalyst has the following structure:

wherein,

M is ruthenium or osmium;

X and X 1 are each independently an anionic ligand;

L is a neutral electron donor ligand; and

R, R 1 , R 6 , R 7 , R 8 , and R 9 are each independently hydrogen, C 1-10 alkyl, C 2-20 alkenyl, C 2-20 alkynyl, aryl, C 1-20 carboxylate, C 1-20 alkoxy, C 2-20 alkenyloxy, C 2-20 alkynyloxy, aryloxy, C 2-20 alkoxycarbonyl, C 1-20 alkylthiol, aryl thiol, C 1-20 alkylsulfonyl, and C 1-20 alkylsulfinyl, and wherein each of R and R 1 is optionally substituted with halogen, C 1-10 alkyl, C 1-10 alkoxy, aryl, hydroxyl, thiol, thioether, ketone, aldehyde, ester, ether, amino, amido, imino, nitro, carboxylic acid, disulfide, carbonate, isocyanate, carbodiimide, carboalkoxy, or carbamate.

9. The metathesis catalyst of claim 8 , wherein at least one of L, L 1 , R, R 1 , R 8 , R 9 , X, and X 1 is linked with at least one of L, L 1 , R, R 1 , R 8 , R 9 , X, and X 1 to form a bonded, bidentate, or multidentate ligand array.

10. The metathesis catalyst of claim 8 , wherein L is bonded together with one of X and X 1 to form a bidentate ligand.

11. The metathesis catalyst of claim 8 , wherein L is bonded together with one of R and R 1 to form a bidentate ligand.

12. The metathesis catalyst of claim 8 , wherein R and R 1 are bonded together.

13. A metathesis catalyst wherein the metathesis catalyst has the following structure:

wherein,

M is Ru or Os;

X and X 1 are each independently an anionic ligand;

P is phosphorus;

R g , R h and R i are each independently:

(1) a C 1-10 alkyl group,

(2) a C 3-10 cycloalkyl group or

(3) a C 5-20 aryl group;

R, R 6 , R 7 , R 8 , and R 9 are each independently:

(1) hydrogen,

(2) a C 1-10 alkyl group,

(3) a C 2-20 alkenyl group,

(4) a C 2-20 alkynyl group,

(5) an aryl group,

(6) a C 1-20 carboxyiate group,

(7) a C 1-20 alkoxy group,

(8) a C 2-20 alkenyloxy group,

(9) a C 2-20 alkynyloxy group,

(10) an aryloxy group,

(11) a C 2-20 alkoxycarbonyl group,

(12) a C 1-20 alkylthiol group,

(13) a C 1-20 alkylsulfonyl group,

(14) a C 1-20 alkylsulfinyl group,

where each of R, R 6 , R 7 , R 8 , and R 9 is optionally substituted with

(a) halogen,

(h) a C 1-10 alkyl group,

(c) a C 1-10 alkoxy group,

(d) an aryl group

(e) a hydroxyl group,

(f) a thiol group,

(g) a thioester group,

(h) a ketone group,

(i) an aldehyde group,

(j) an ester group,

(k) an ether group,

(l) an amino group,

(m) an amido group,

(n) an imino group,

(o) a nitro group,

(p) a carboxylic acid group,

(q) a disulfide group,

(r) a carbonate group,

(s) an isocyanate group,

(t) a carbodiimide group,

(u) a carboalkoxy group, or

(v) a carbamate group.

Assignments (2)
CONFIRMATORY LICENSE Recorded Nov 21, 2013
From: CALIFORNIA INSTITUTE OF TECHNOLOGY
To: NATIONAL INSTITUTES OF HEALTH (NIH), U.S. DEPT. OF HEALTH AND HUMAN SERVICES (DHHS), U.S. GOVERNMENT
Reel/Frame 031694/0014 →
CONFIRMATORY LICENSE Recorded Nov 21, 2013
From: CALIFORNIA INSTITUTE OF TECHNOLOGY
To: NATIONAL INSTITUTES OF HEALTH (NIH), U.S. DEPT. OF HEALTH AND HUMAN SERVICES (DHHS), U.S. GOVERNMENT
Reel/Frame 031694/0016 →
Continuity (5)
Continuation 12016482 · Jan 18, 2008
Division 09576370 · May 22, 2000
Provisional Application 60142853 · Jul 7, 1999
Provisional Application 60135493 · May 24, 1999
Related Publication 20130165661A1 · Jun 27, 2013