IP Library Granted Patent US 9,624,338
Granted Patent B2
US 9,624,338 · App. 14/906,834 · Granted Apr 18, 2017

Alternating ring-opening metathesis polymerization

Inventors: Nicole S. Sampson (Setauket, NY); Li Tan (Centereach, NY); Kathlyn Parker (Setauket, NY)
Assignee: The Research Foundation for The State University of New York
C08G61/08A61K9/1075A61K31/74A61K47/32A61K47/48176C08F232/04C08G61/128C09D5/1637C08G61/12C08G2261/124C08G2261/418C08G2261/74
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Quick Facts
Patent No.
US 9,624,338
App. No.
14/906,834
Granted
Apr 18, 2017
Kind
B2
Abstract

The invention relates to the field of polymers and olefin polymerization, and more specifically olefin metathesis polymerization. The invention provides regioregular alternating polymers and methods of synthesizing such polymers. To demonstrate, polymers were synthesized and modified with a FRET pair (Trp/Dansyl) post-polymerization.

Claims (24)

1. A method for producing a polymer comprising the repeating unit (Ib) or (Ic):

which comprises contacting an olefin of structure (II) with a cyclobutene of structure (III)

in the presence of an olefin metathesis catalyst, wherein

R is selected from the group consisting of H, C 1 -C 20 alkyl, C 2 -C 20 alkenyl, C 3 -C 8 cycloalkyl, heterocyclyl, aryl, C 1 -C 20 alkoxy, C 1 -C 20 alkenyloxy, C 3 -C 6 cycloalkyloxy, aryloxy, heterocyclyloxy, C 1 -C 20 alkylamino, C 1 -C 20 alkenylamino, C 3 -C 8 cycloalkylamino, heterocyclylamino, or arylamino and may be optionally substituted with up to three substituents selected from halo, CN, NO 2 , oxo, alkyl, cycloalkyl, alkenyl, alkynyl, aralkyl, aryl, and a heterocyclic group;

n is a number between 2 and 20;

R 1 through R 6 are independently selected from the group consisting of H, aldehyde, C 1 -C 20 alkyl, C 2 -C 20 alkenyl, C 3 -C 6 cycloalkyl, aryl, heterocyclyl, C 1 -C 20 alkoxy, C 1 -C 20 acyloxy, C 2 -C 20 alkenyloxy, C 3 -C 6 cycloalkyloxy, aryloxy, heterocyclyloxy, C 1 -C 20 alkylamino, C 2 -C 20 alkenylamino, C 3 -C 8 cycloalkylamino, heterocyclylamino, arylamino, or halogen;

R 1 through R 6 may be taken together to form a 5- to 7-membered ring which may be optionally substituted with up to three substituents selected from halo, CN, NO 2 , oxo, alkyl, cycloalkyl, alkenyl, alkynyl, aralkyl, aryl, or a heterocyclic group;

A is a C 2 -C 20 alkyl;

with the proviso that any carbon-carbon double bonds in R or in R 1 through R 6 are essentially unreactive toward metathesis reactions with the catalyst.

2. The method of claim 1 , further comprising combining a polymer block comprising repeating units (Ib) or (Ic) into a block copolymer.

3. The method of claim 1 , wherein the catalyst is an alkylidene ruthenium complex of formula (L)(L′)X 2 Ru=CHR′ or (L) 2 (L′)X 2 Ru═CHR′, wherein R′ is selected from the group consisting of H, C 1 -C 10 alkyl, C 2 -C 10 alkenyl, C 3 -C 6 cycloalkyl, and aryl;

L is a ligand selected from the group consisting of trialkyl phosphines, triarylphosphines, tri(cycloalkyl)phosphines, pyridine and substituted pyridine;

L′ is a ligand selected from the group consisting of trialkyl phosphines, triarylphosphines, tri(cycloalkyl)phosphines, pyridine and substituted pyridine, and imidazolin-2-ylidine carbenes of formula

wherein Ar is an ortho-substituted aryl or an aryl; and

X is F, Cl, or Br.

4. The method of claim 2 , wherein the catalyst is an alkylidene ruthenium complex of formula (L)(L′)X 2 Ru═CHR′ or (L) 2 (L′)X 2 Ru═CHR′, wherein R′ is selected from the group consisting of H, C 1 -C 10 alkyl, C 2 -C 10 alkenyl, C 3 -C 6 cycloalkyl, and aryl;

L is a ligand selected from the group consisting of trialkyl phosphines, triarylphosphines, tri(cycloalkyl)phosphines, pyridine and substituted pyridine;

L′ is a ligand selected from the group consisting of trialkyl phosphines, triarylphosphines, tri(cycloalkyl)phosphines, pyridine and substituted pyridine, and imidazolin-2-ylidine carbenes of formula

wherein Ar is an ortho-substituted aryl or an aryl; and

X is F, Cl, or Br.

5. The method of claim 3 , wherein L is pyridine or substituted pyridine.

6. The method of claim 4 , wherein L is 3-bromopyridyl, 3-chloropyridyl or pyridine.

7. The method of claim 3 , wherein L′ is an imidazolin-2-ylidine carbene and Ar is selected from the group consisting of phenyl, mesityl, 2-methylphenyl, 2-ethylphenyl, 2-isopropylphenyl, 2,3-diisopropylphenyl, 2,6-difluorophenyl, and 3,5-di-t-butylphenyl.

8. The method of claim 1 , wherein the catalyst is a molybdenum or tungsten metathesis catalyst.

Assignments (2)
CONFIRMATORY LICENSE Recorded Dec 12, 2017
From: STATE UNIVERSITY NEW YORK STONY BROOK
To: NATIONAL INSTITUTES OF HEALTH (NIH), U.S. DEPT. OF HEALTH AND HUMAN SERVICES (DHHS), U.S. GOVERNMENT
Reel/Frame 044836/0372 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Dec 19, 2016
From: SAMPSON, NICOLE S.; TAN, LI; PARKER, KATHLYN
To: THE RESEARCH FOUNDATION FOR THE STATE UNIVERSITY OF NEW YORK
Reel/Frame 040671/0359 →
Continuity (3)
Provisional Application 61857189 · Jul 22, 2013
Provisional Application 61858811 · Jul 26, 2013
Related Publication 20160159972A1 · Jun 9, 2016