IP Library Granted Patent US 9,079,173
Granted Patent B2
US 9,079,173 · App. 13/751,815 · Granted Jul 14, 2015

Highly

Inventors: Richard R. Schrock (Winchester, MA); Annie J. King (Cambridge, MA); Yu Zhao (Brighton, MA); Margaret M. Flook (Cambridge, MA); Amir H. Hoveyda (Lincoln, MA)
Assignees: Massachusetts Institute of Technology; Trustee of Boston College
B01J31/2295B01J31/181B01J31/1805B01J31/1825B01J31/2226B01J31/2265C07C6/04C07C41/30C07C67/475C07C209/68C07C303/40C07F7/083C07F11/005B01J2231/543B01J2531/0266B01J2531/0288B01J2531/64B01J2531/66B01J2540/225C07B2200/09C07C2101/14C07C2531/22
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Quick Facts
Patent No.
US 9,079,173
App. No.
13/751,815
Granted
Jul 14, 2015
Kind
B2
Abstract

The present invention relates generally to catalysts and processes for the Z-selective formation of internal olefin(s) from terminal olefin(s) via homo-metathesis reactions.

Claims (39)

1. A metal complex having the structure:

wherein:

M is Mo or W;

R 1 is aryl, heteroaryl, alkyl, or heteroalkyl, optionally substituted;

R 2 and R 3 can be the same or different and are hydrogen, alkyl, alkenyl, heteroalkyl, heteroalkenyl, aryl, or heteroaryl, optionally substituted; and

R 4 and R 5 can be the same or different and are alkyl, heteroalkyl, aryl, heteroaryl, silylalkyl, or silyloxy, optionally substituted, wherein at least one of R 4 or R 5 is a ligand containing oxygen bound to M, and

wherein the ligand containing oxygen bound to M is hexaisopropylterphenolate (O-2,6-(2,4,6-i-Pr 3 C 6 H 2 ) 2 C 6 H 3 ).

2. The metal complex of claim 1 , wherein one of R 4 and R 5 is hexaisopropylterphenolate, and the other is a ligand containing nitrogen bound to M, optionally substituted.

3. The metal complex of claim 1 , wherein the metal complex is other than Mo(NAd)(CHCMe 2 Ph)(Pyr)(HIPTO), Mo(NAd)(CHCMe 2 Ph)(Me 2 Pyr)(HIPTO), Mo(NAr)(CHCMe 2 Ph)(Pyr)(HIPTO), and W(NAr)(CHCMe 2 Ph)(Pyr)(HIPTO), wherein Ad is 1-adamantyl, Ar is 2,6-i-Pr 2 C 6 H 3 , Pyr is pyrrolide, Me 2 Pyr is 2,5-dimethylpyrrolide, and HIPTO is (O-2,6-(2,4,6-i-Pr 3 C 6 H 2 ) 2 C 6 H 3 .

4. The metal complex of claim 2 , wherein the ligand containing nitrogen bound to M is selected from the group consisting of pyrrolyl, pyrazolyl, pyridinyl, pyrazinyl, pyrimidinyl, imidazolyl, triazolyl, tetrazolyl, oxazolyl, isoxazolyl, thiazolyl, isothiazolyl, indolyl, indazolyl, carbazolyl, morpholinyl, piperidinyl, and oxazinyl, all optionally substituted.

5. The metal complex of claim 2 , wherein the ligand containing nitrogen bound to M is pyrrolyl, optionally substituted.

6. The metal complex of claim 2 , wherein M is Mo.

7. The metal complex of claim 2 , wherein R 1 and R 2 are the same or different and are aryl or alkyl, optionally substituted, and R 3 is hydrogen.

8. The metal complex of claim 2 , wherein the ligand containing nitrogen bound to M has the structure:

wherein each R 6 can be the same or different and is hydrogen, alkyl, heteroalkyl, aryl, or heteroaryl, optionally substituted; and

X may be present or absent and is any non-interfering group.

9. The metal complex of claim 6 , wherein R 1 is not 1-adamantyl or 2,6-i-Pr 2 C 6 H 3 .

10. The metal complex of claim 2 , wherein M is W.

11. The metal complex of claim 1 , wherein R 1 is:

wherein each R 17 can be the same or different and is hydrogen, halogen, alkyl, heteroalkyl, aryl, acyl, or —OP, optionally substituted; and

P is a protecting group.

12. The metal complex of claim 1 , wherein R 1 is:

wherein each R 17 can be the same or different and is hydrogen, halogen, alkyl, heteroalkyl, aryl, acyl, or —OP, optionally substituted; and

P is a protecting group.

13. The metal complex of claim 1 , wherein R 2 is alkyl.

14. The metal complex of claim 10 , wherein R 1 is not 2,6-i-Pr 2 C 6 H 3 .

15. The metal complex of claim 2 , wherein ═CR 2 R 3 is not ═CHCMe 2 Ph.

16. The metal complex of claim 1 , wherein R 2 is CMe 2 Ph or CMe 3 and R 3 is hydrogen.

17. The metal complex of claim 1 , wherein M is W and R 1 is not:

18. The metal complex of claim 1 , wherein M is W and R 1 is:

wherein each R 17 can be the same or different and is hydrogen, halogen, alkyl, heteroalkyl, aryl, acyl, or —OP, optionally substituted, and P is a protecting group.

19. The metal complex of claim 1 , wherein the metal complex has a structure selected from the group consisting of M(NAr)(Pyr)(CHR 2 )(HIPTO), M(NAr Cl )(CHCMe 3 )(Me 2 Pyr)(HIPTO), M(NAr Cl )(CHCMe 3 )(Me 2 Pyr)(HIPTO), M(NAd)(CHCMe 2 Ph)(Me 2 Pyr)(HIPTO), M(NAr′)(Pyr)(CHR 2 )(HIPTO), and M(NAr′)(CHCMe 2 Ph)(Me 2 Pyr)(HIPTO), wherein M is Mo or W, Ar is 2,6-diisopropylphenyl, Ar Cl is 2,6-dichlorophenyl, Ar′ is 2,6-dimethyphenyl, Ad is 1-adamantyl, Me 2 Pyr is 2,5-dimethylpyrrolide, Pyr is pyrrolide, and HIPTO is hexaisopropylterphenolate, OSi(TMS).

20. The metal complex of claim 1 , wherein the heteroalkyl is an alkoxy.

21. The metal complex of claim 1 , wherein the heteroaryl is an aryloxy.

22. The metal complex of claim 2 , wherein R 2 is CMe 3 and R 3 is hydrogen.

23. The metal complex of claim 19 , wherein the metal complex has a structure selected from the group consisting of M(NAr Cl )(CHCMe 3 )(Me 2 Pyr)(HIPTO), M(NAr Cl )(CHCMe 3 )(Me 2 Pyr)(HIPTO), M(NAr′)(Pyr)(CHR 2 )(HIPTO) and M(NAr′)(CHCMe 2 Ph)(Me 2 Pyr)(HIPTO).

24. The metal complex of claim 1 , wherein the metal complex is selected from W(NAr)(Pyr)(CHCMe 2 Ph)(HIPTO), W(NAr′)(CHCMe 2 Ph)(Pyr)(HIPTO), W(NAr Cl )(CHCMe 3 )(Pyr)(HIPTO), Mo(NAd)(CHCMe 3 )(Pyr)(HIPTO), Mo(NAd)(CHCMe 2 Ph)(Pyr)(HIPTO), W(NAr Cl )(CHMe 3 )(Pyr)(HIPTO), W(NAr′)(CHCMe 2 Ph)(Me 2 Pyr)(HIPTO), Mo(NAd)(CHCMe 2 Ph)(Me 2 Pyr)(HIPTO), W(NAr Cl )(CHCMe 3 )(Pyr)(HIPTO), W(NAr′)(CHCMe 2 Ph)(Pyr)(HIPTO), and Mo(NAr)(CHCMe 2 Ph)(Pyr)(HIPTO).

25. The metal complex of claim 1 , wherein the metal complex is selected from W(NAr′)(CHCMe 2 Ph)(Pyr)(HIPTO), W(NAr Cl )(CHCMe 3 )(Pyr)(HIPTO), Mo(NAd)(CHCMe 3 )(Pyr)(HIPTO), W(NAr Cl )(CHMe 3 )(Pyr)(HIPTO), W(NAr′)(CHCMe 2 Ph)(Me 2 Pyr)(HIPTO), W(NAr Cl )(CHCMe 3 )(Pyr)(HIPTO), and W(NAr′)(CHCMe 2 Ph)(Pyr)(HIPTO).

26. The metal complex of claim 3 , wherein the ligand containing nitrogen bound to M is pyrrolyl, optionally substituted.

Assignments (3)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 28, 2014
From: SCHROCK, RICHARD R.; KING, ANNIE J.; ZHAO, YU; FLOOK, MARGARET M.
To: MASSACHUSETTS INSTITUTE OF TECHNOLOGY
Reel/Frame 032977/0524 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 23, 2013
From: HOVEYDA, AMIR H.
To: TRUSTEES OF BOSTON COLLEGE
Reel/Frame 030853/0414 →
CONFIRMATORY LICENSE Recorded Mar 8, 2013
From: MASSACHUSETTS INSTITUTE OF TECHNOLOGY
To: NATIONAL INSTITUTES OF HEALTH (NIH), U.S. DEPT. OF HEALTH AND HUMAN SERVICES (DHHS), U.S. GOVERNMENT
Reel/Frame 029942/0371 →
Continuity (1)
Related Publication 20130274482A1 · Oct 17, 2013