IP Library Granted Patent US 9,403,753
Granted Patent B2
US 9,403,753 · App. 14/948,898 · Granted Aug 2, 2016

Dual site catalyst for mild, selective nitrile reduction

Inventors: Travis J. Williams (Los Angeles, CA); Zhiyao Lu (Los Angeles, CA)
Assignee: University of Southern California
C07C209/48B01J31/181C07C213/02C07D213/38C07D307/68C07D333/38C07F15/0046B01J2231/64B01J2531/821
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Quick Facts
Patent No.
US 9,403,753
App. No.
14/948,898
Granted
Aug 2, 2016
Kind
B2
Abstract

A ruthenium bis(pyrazolyl)borate scaffold that enables cooperative reduction reactivity in which boron and ruthenium centers work in concert to effect selective nitrile reduction is provided. The pre-catalyst compound [κ 3 -(1-pz) 2 HB(N═CHCH 3 )]Ru(cymene) + TfO − (pz=pyrazolyl) was synthesized using readily-available materials through a straightforward route, thus making it an appealing catalyst for a number of reactions.

Claims (45)

1. A compound having formula I:

wherein:

R 1 are each independently hydrogen, C 1-8 alkyl, chlorine, bromine, fluorine, or OH;

x is 0 to 3;

R 2 is C 6-12 aryl, C 5-12 heteroaryl or C 1-8 alkyl;

L 1 are each independently ligands associated with M, each L 1 are the same or different; and

a is an integer from 1 to 6; and

M is a transition metal.

2. The compound of claim 1 having formula II:

wherein:

R 1 are each independently hydrogen, C 1-8 alkyl, chlorine, bromine, fluorine, or OH;

x is 0 to 3;

R 2 is C 6-12 aryl, C 5-12 heteroaryl or C 1-8 alkyl;

R 3 are each independently hydrogen, C 1-8 alkyl, chlorine, bromine, fluorine, or OH;

z is 0 to 4; and

M is a transition metal.

3. The compound of claim 1 having the following formula:

4. The compound of claim 1 wherein M is a metal selected from the group consisting of beryllium, magnesium, aluminum, scandium, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, zinc, gallium, germanium, yttrium, zirconium, niobium, molybdenum, technetium, ruthenium, rhodium, palladium, silver, cadmium, indium, tin, antimony, lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, hafnium, tantalum, tungsten, rhenium, osmium, iridium, gold, platinum, thallium, lead, bismuth, polonium, thorium, protactinium, uranium, neptunium, and plutonium.

5. The compound of claim 1 wherein M is ruthenium.

6. The compound of claim 1 wherein the L 1 are each independently selected from the group consisting of neutral two electron donor ligands, anionic two electron donor ligands, pi-donor ligands, multidentate ligands, and monodentate ligands.

7. The compound of claim 1 wherein the L 1 are each independently selected from the group consisting of substituted or unsubstituted phenyl, carbon dioxide, halide, hydride, nitrate, hydroxide, acetonitrile, pyridine, ammonia, aquo, boryl, and combinations thereof.

8. The compound of claim 1 wherein the R 1 are each independently hydrogen, methyl, ethyl, n-propyl, isopropyl, n-butyl, sec-butyl, isobutyl, or t-butyl.

9. The compound of claim 2 wherein the R 3 are each independently hydrogen, methyl, ethyl, n-propyl, isopropyl, n-butyl, sec-butyl, isobutyl, or t-butyl.

10. The compound of claim 1 wherein the R 2 are each independently methyl, ethyl, n-propyl, isopropyl, n-butyl, sec-butyl, isobutyl, or t-butyl.

11. A method comprising:

contacting a compound having a reducible functional group with a metal-containing compound having formula I or II and a reducing agent:

the reducible functional group being a cyano group, aldehyde group, and/or ketone group,

wherein:

R 1 are each independently hydrogen, C 1-8 alkyl, chlorine, bromine, fluorine, or OH;

R 2 is C 6-12 aryl, C 5-12 heteroaryl or C 1-8 alkyl;

R 3 are each independently hydrogen, C 1-8 alkyl, chlorine, bromine, fluorine, or OH;

L 1 are each independently ligands associated with M, each L 1 are the same or different;

a is an integer from 1 to 6;

x is 0 to 3;

z is 0 to 4; and

M is a transition metal.

12. The method of claim 11 wherein the reducing agent is selected form the group consisting of NaBH 4 , alcohols, and formic acid.

13. The method of claim 11 wherein the reducible functional group is a cyano group.

14. The method of claim 11 wherein the reducible functional group is a C 2-12 aldehyde and/or a C 3-12 aldehyde.

15. The method of claim 11 wherein M is a metal selected from the group consisting of beryllium, magnesium, aluminum, scandium, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, zinc, gallium, germanium, yttrium, zirconium, niobium, molybdenum, technetium, ruthenium, rhodium, palladium, silver, cadmium, indium, tin, antimony, lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, hafnium, tantalum, tungsten, rhenium, osmium, iridium, gold, platinum, thallium, lead, bismuth, polonium, thorium, protactinium, uranium, neptunium, and plutonium.

16. The method of claim 11 wherein M is ruthenium.

17. The method of claim 11 wherein the L 1 are each independently selected from the group consisting of neutral two electron donor ligands, anionic two electron donor ligands, pi-donor ligands, multidentate ligands, and monodentate ligands.

18. The method of claim 11 wherein the L 1 are each independently selected from the group consisting of substituted or unsubstituted phenyl, carbon dioxide, halide, hydride, nitrate, hydroxide, acetonitrile, pyridine, ammonia, aquo, boryl, and combinations thereof.

19. The method of claim 11 wherein the R 1 are each independently hydrogen, methyl, ethyl, n-propyl, isopropyl, n-butyl, sec-butyl, isobutyl, or t-butyl.

20. The method of claim 11 wherein the R 2 and the R 3 are each independently methyl, ethyl, n-propyl, isopropyl, n-butyl, sec-butyl, isobutyl, or t-butyl.

Assignments (2)
CONFIRMATORY LICENSE Recorded Apr 15, 2020
From: UNIVERSITY OF SOUTHERN CALIFORNIA
To: NATIONAL SCIENCE FOUNDATION
Reel/Frame 052406/0439 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 13, 2016
From: WILLIAMS, TRAVIS J.; LU, ZHIYAO
To: UNIVERSITY OF SOUTHERN CALIFORNIA
Reel/Frame 037478/0826 →
Continuity (2)
Provisional Application 62082992 · Nov 21, 2014
Related Publication 20160145193A1 · May 26, 2016