IP Library Granted Patent US 9,688,789
Granted Patent B2
US 9,688,789 · App. 14/305,039 · Granted Jun 27, 2017

Degradable polycations derived from amino acid vinyl esters

Inventors: Mahesh Kalyana Mahanthappa (Madison, WI); Glen Bradley Thomas (Madison, WI); Corinne Elizabeth Lipscomb (St. Paul, MN)
Assignee: NATIONAL SCIENCE FOUNDATION
C08F26/06C08F22/26C08F26/02C08F216/1458C08F218/08C08F226/02C08F226/06C08F18/04C08F18/22C08F218/04C08F218/10
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Quick Facts
Patent No.
US 9,688,789
App. No.
14/305,039
Granted
Jun 27, 2017
Kind
B2
Abstract

Described herein are the synthesis and polymerization of a series of N-Boc-protected amino acid vinyl ester (BAAVE) monomers. Homopolymers and heteropolymers containing the monomers are described, particularly heteropolymers with vinyl ester monomers such as vinyl acetate. Deprotection can be used to produce hydrophilic and hydrophobic polymers that are particular useful in biological applications such as cellular delivery of biological materials.

Claims (64)

1. A copolymer consisting of units of the formula

and salts thereof, wherein

R t is H, halo, or methyl,

Q is cyano, halo, nitro, OH, —CR a ═CR b R c , —C(O)NR d R e , carbonyl(C 1 -C 12 )alkyl, substituted or unsubstituted C 6 -C 12 aryl, N-caprolactam, or a combination comprising at least one of the foregoing groups, wherein each R a , R b , and R c are independently H or C 1 -C 18 alkyl, and wherein each R d and R e are independently H or C 1 -C 18 alkyl,

x+y is an integer greater than two,

R is H, a substituted or unsubstituted C 1 -C 18 alkyl, a substituted or unsubstituted C 2 -C 18 alkenyl, a substituted or unsubstituted C 2 -C 18 alkynyl, a substituted or unsubstituted C 3 -C 18 cycloalkyl, a substituted or unsubstituted C 1 -C 18 haloalkyl, a substituted or unsubstituted C 2 -C 18 heterocycloalkyl, a substituted or unsubstituted C 6 -C 18 aryl, a substituted or unsubstituted C 7 -C 18 arylalkylene, or a substituted or unsubstituted C 3 -C 18 heteroaryl;

R′ is a substituted or unsubstituted C 1 -C 18 alkyl, a substituted or unsubstituted C 2 -C 18 alkenyl, a substituted or unsubstituted C 2 -C 18 alkynyl, a substituted or unsubstituted C 3 -C 18 cycloalkyl, a substituted or unsubstituted C 1 -C 18 haloalkyl, a substituted or unsubstituted C 2 -C 18 heterocycloalkyl, a substituted or unsubstituted C 6 -C 18 aryl, a substituted or unsubstituted C 7 -C 18 arylalkylene, or a substituted or unsubstituted C 3 -C 18 heteroaryl, wherein substituted for R′ comprises replacement of one or more hydrogen atoms of a group with a substituent selected from a C 1 to C 6 alkyl group; a C 1 to C 6 hydroxyalkyl group; a C 2 to C 6 alkenyl group; a C 2 to C 30 alkynyl group; a C 6 to C 30 aryl group; a C 1 to C 6 heteroalkyl group; a C 3 to C 30 cycloalkyl group; a C 3 to C 15 cycloalkenyl group; a C 6 to C 30 cycloalkynyl group; a C 2 to C 30 heterocycloalkyl group; halogen; a haloalkyl group; an alkoxy group; —NO 2 ; —CN; —NR′″ 2 wherein each R″′ is independently a hydrogen or a C 1 to C 6 alkyl group, a C 2 to C 6 alkynyl group, or a C 6 to C 30 aryl group; a carbamyl group; —C(═O)OR″ wherein R″ is a C 1 to C 6 alkyl group or a C 6 to C 10 aryl group; or —C(═O)OH; and

G is a group of the formula

 wherein

one of *′ and *″ indicates a point of attachment to the carbonyl and the other indicates a point of attachment to N, and *′″ indicates a point of attachment to R,

z is 0, 1, or 2, and

R w , R x and R y are each independently H, a substituted or unsubstituted C 1 -C 18 alkyl, a substituted or unsubstituted C 2 -C 18 alkenyl, a substituted or unsubstituted C 2 -C 18 alkynyl, a substituted or unsubstituted C 3 to C 18 cycloalkyl, a substituted or unsubstituted C 1 -C 18 haloalkyl, a substituted or unsubstituted C 2 -C 18 heterocycloalkyl, a substituted or unsubstituted C 6 to C 18 aryl, a substituted or unsubstituted C 7 to C 18 arylalkylene, or a substituted or unsubstituted C 4 -C 18 heteroaryl, or any two of R, R′, R w , R x , and R y together form a substituted or unsubstituted C 5 -C 18 cycloalkyl, substituted or unsubstituted C 2 -C 18 heterocycloalkyl, or substituted or unsubstituted C 2 -C 18 heteroaryl group, each having 5 to 8 ring members.

2. A copolymer consisting of units of the formula

and salts thereof, wherein

R t is H, halo, or methyl,

Q is cyano, halo, nitro, OH, —CR a ═CR b R c , —C(O)NR d R e , carbonyl(C 1 -C 12 )alkyl, carbonyloxy(C 1 -C 12 )alkyl, substituted or unsubstituted C 6 -C 12 aryl, N-caprolactam, or a combination comprising at least one of the foregoing groups, wherein each R a , R b , and R c are independently H or C 1 -C 18 alkyl, and wherein each R d and R e are independently H or C 2 -C 18 alkyl, carbonyl(C 1 -C 12 )alkyl,

x+y is an integer greater than two,

z is 0, 1, or 2, and

R′ together with R forms a substituted or unsubstituted C 2 -C 18 heterocycloalkyl, or substituted or unsubstituted C 2 -C 18 heteroaryl group, each having 5 to 8 ring members.

3. The copolymer of claim 2 , wherein R and R′ together form propylene to provide a monomer having a 5-membered ring.

4. The copolymer of claim 2 , wherein Q is carbonyl(C 1 -C 12 )alkyl, carbonyloxy(C 1 -C 12 )alkyl, substituted or unsubstituted C 6 -C 12 aryl, N-caprolactam, or a combination comprising at least one of the foregoing groups.

5. A copolymer consisting of units of the formula

and salts thereof, wherein

R t is halo,

Q is cyano, halo, nitro, OH, —CR a ═CR b R c , —C(O)NR d R e , carbonyl(C 1 -C 12 )alkyl, carbonyloxy(C 1 -C 12 )alkyl-substituted or unsubstituted C 6 -C 12 aryl, N-caprolactam, or a combination comprising at least one of the foregoing groups, wherein each R a , R b , and R c are independently H or C 1 -C 18 alkyl, and wherein each R d and R e are independently H or C 1 -C 18 alkyl,

x+y is an integer greater than two,

R is H, a substituted or unsubstituted C 1 -C 18 alkyl, a substituted or unsubstituted C 2 -C 18 alkenyl, a substituted or unsubstituted C 2 -C 18 alkynyl, a substituted or unsubstituted C 3 -C 18 cycloalkyl, a substituted or unsubstituted C 1 -C 18 haloalkyl, a substituted or unsubstituted C 2 -C 18 heterocycloalkyl, a substituted or unsubstituted C 6 -C 18 aryl, a substituted or unsubstituted C 7 -C 18 arylalkylene, or a substituted or unsubstituted C 3 -C 18 heteroaryl;

R′ is H, a substituted or unsubstituted C 1 -C 18 alkyl, a substituted or unsubstituted C 2 -C 18 alkenyl, a substituted or unsubstituted C 2 -C 18 alkynyl, a substituted or unsubstituted C 3 -C 18 cycloalkyl, a substituted or unsubstituted C 1 -C 18 haloalkyl, a substituted or unsubstituted C 2 -C 18 heterocycloalkyl, a substituted or unsubstituted C 6 -C 18 aryl, a substituted or unsubstituted C 7 -C 18 arylalkylene, or a substituted or unsubstituted C 3 -C 18 heteroaryl, wherein substituted for R′ comprises replacement of one or more hydrogen atoms of a group with a substituent selected from a C 1 to C 6 alkyl group; a C 1 to C 6 hydroxyalkyl group; a C 2 to C 6 alkenyl group; a C 2 to C 30 alkynyl group; a C 6 to C 30 aryl group; a C 1 to C 6 heteroalkyl group; a C 3 to C 30 cycloalkyl group; a C 3 to C 15 cycloalkenyl group; a C 6 to C 30 cycloalkynyl group; a C 2 to C 30 heterocycloalkyl group; halogen; a haloalkyl group; an alkoxy group; —NO 2 ; —CN; —NR′″ 2 wherein each R′″ is independently a hydrogen or a C 1 to C 6 alkyl group, a C 2 to C 6 alkynyl group, or a C 6 to C 30 aryl group; a carbamyl group; —C(═O)OR″ wherein R″ is a C 1 to C 6 alkyl group or a C 6 to C 10 aryl group; or —C(═O)OH; and

G is a group of the formula

 wherein

one of *′ and *″ indicates a point of attachment to the carbonyl and the other indicates a point of attachment to N, and *′″ indicates a point of attachment to R,

z is 0, 1, or 2, and

R w R x and R y are each independently H, a substituted or unsubstituted C 1 -C 18 alkyl, a substituted or unsubstituted C 2 -C 18 alkenyl, a substituted or unsubstituted C 2 -C 18 alkynyl, a substituted or unsubstituted C 3 to C 18 cycloalkyl, a substituted or unsubstituted C 1 -C 18 haloalkyl, a substituted or unsubstituted C 2 -C 18 heterocycloalkyl, a substituted or unsubstituted C 6 to C 18 aryl, a substituted or unsubstituted C 7 to C 18 arylalkylene, or a substituted or unsubstituted C 4 -C 18 heteroaryl, or any two of R, R′, R w , R x , and R y together form a substituted or unsubstituted C 5 -C 18 cycloalkyl, substituted or unsubstituted C 2 -C 18 heterocycloalkyl, or substituted or unsubstituted C 2 -C 18 heteroaryl group, each having 5 to 8 ring members.

6. A copolymer consisting of units of the formula

and salts thereof, wherein

R t is halo,

Q is cyano, halo, nitro, OH, —CR a ═CR b R c , —C(O)NR d R e , carbonyl(C 1 -C 12 )alkyl, carbonyloxy(C 1 -C 12 )alkyl, substituted or unsubstituted C 6 -C 12 aryl, N-caprolactam, or a combination comprising at least one of the foregoing groups, wherein each R a , R b , and R c are independently H or C 1 -C 18 alkyl, and wherein each R d and R e are independently H or C 1 -C 18 alkyl, carbonyl(C 1 -C 12 )alkyl,

x+y is an integer greater than two,

z is 0, 1, or 2, and

R is H, a substituted or unsubstituted C 1 -C 18 alkyl, a substituted or unsubstituted C 2 -C 18 alkenyl, a substituted or unsubstituted C 2 -C 18 alkynyl, a substituted or unsubstituted C 3 -C 18 cycloalkyl, a substituted or unsubstituted C 1 -C 18 haloalkyl, a substituted or unsubstituted C 2 -C 18 heterocycloalkyl, a substituted or unsubstituted C 6 -C 18 aryl, a substituted or unsubstituted C 7 -C 18 arylalkylene, or a substituted or unsubstituted C 3 -C 18 heteroaryl, R′ is H or R′ together with R forms a substituted or unsubstituted C 2 -C 18 heterocycloalkyl, or substituted or unsubstituted C 2 -C 18 heteroaryl group, each having 5 to 8 ring members.

7. The copolymer of claim 6 , wherein R is H, methyl, ethyl, propyl, isopropyl, butyl, isobutyl, sec-butyl, methylthiomethylene, benzyl, indolylmethylene, or R and R′ together form propylene to provide a monomer having a 5-membered ring.

8. The copolymer of claim 6 , wherein Q is carbonyl(C 1 -C 12 )alkyl, carbonyloxy(C 1 -C 12 )alkyl, substituted or unsubstituted C 6 -C 12 aryl, N-caprolactam, or a combination comprising at least one of the foregoing groups.

9. A copolymer consisting of units of the formula

and salts thereof, wherein

R t is H, halo, or methyl,

Q is cyano, halo, nitro, OH, —CR a ═CR b R c , —C(O)NR d R e , carbonyl(C 1 -C 12 )alkyl, substituted or unsubstituted C 6 -C 12 aryl, or a combination comprising at least one of the foregoing groups, wherein each R a , R b , and R c are independently H or C 1 -C 18 alkyl, and wherein each R d and R e are independently H or C 1 -C 18 alkyl,

x+y is an integer greater than two,

R is H, a substituted or unsubstituted C 1 -C 18 alkyl, a substituted or unsubstituted C 2 -C 18 alkenyl, a substituted or unsubstituted C 2 -C 18 alkynyl, a substituted or unsubstituted C 3 -C 18 cycloalkyl, a substituted or unsubstituted C 1 -C 18 haloalkyl, a substituted or unsubstituted C 2 -C 18 heterocycloalkyl, a substituted or unsubstituted C 6 -C 18 aryl, a substituted or unsubstituted C 7 -C 18 arylalkylene, or a substituted or unsubstituted C 3 -C 18 heteroaryl;

R′ is H, a substituted or unsubstituted C 1 -C 18 alkyl, a substituted or unsubstituted C 2 -C 18 alkenyl, a substituted or unsubstituted C 2 -C 18 alkynyl, a substituted or unsubstituted C 3 -C 18 cycloalkyl, a substituted or unsubstituted C 1 -C 18 haloalkyl, a substituted or unsubstituted C 2 -C 18 heterocycloalkyl, a substituted or unsubstituted C 6 -C 18 aryl, a substituted or unsubstituted C 7 -C 18 arylalkylene, or a substituted or unsubstituted C 3 -C 18 heteroaryl, wherein substituted for R′ comprises replacement of one or more hydrogen atoms of a group with a substituent selected from a C 1 to C 6 alkyl group; a C 1 to C 6 hydroxyalkyl group; a C 2 to C 6 alkenyl group; a C 2 to C 30 alkynyl group; a C 6 to C 30 aryl group; a C 1 to C 6 heteroalkyl group; a C 3 to C 30 cycloalkyl group; a C 3 to C 15 cycloalkenyl group; a C 6 to C 30 cycloalkynyl group; a C 2 to C 30 heterocycloalkyl group; halogen; a haloalkyl group; an alkoxy group; —NO 2 ; —CN)′ NR′″ 2 wherein each R′″ is independently a hydrogen or a C 1 to C 6 alkyl group, a C 2 to C 6 alkynyl group, or a C 6 to C 30 aryl group; a carbamyl group; —C(═O)OR″ wherein R″ is a C 1 to C 6 alkyl group or a C 6 to C 10 aryl group; or —C(═O)OH; and

G is a group of the formula

 wherein

one of *′ and *″ indicates a point of attachment to the carbonyl and the other indicates a point of attachment to N, and *′″ indicates a point of attachment to R,

z is 0, 1, or 2, and

R w , R x and R y are each independently H, a substituted or unsubstituted C 1 -C 18 alkyl, a substituted or unsubstituted C 2 -C 18 alkenyl, a substituted or unsubstituted C 2 -C 18 alkynyl, a substituted or unsubstituted C 3 to C 18 cycloalkyl, a substituted or unsubstituted C 1 -C 18 haloalkyl, a substituted or unsubstituted C 2 -C 18 heterocycloalkyl, a substituted or unsubstituted C 6 to C 18 aryl, a substituted or unsubstituted C 7 to C 18 arylalkylene, or a substituted or unsubstituted C 4 -C 18 heteroaryl, or any two of R, R′, R w , R x , and R y together form a substituted or unsubstituted C 5 -C 18 cycloalkyl, substituted or unsubstituted C 2 -C 18 heterocycloalkyl, or substituted or unsubstituted C 2 -C 18 heteroaryl group, each having 5 to 8 ring members.

10. A copolymer consisting of units of the formula

and salts thereof, wherein

R t is H, halo, or methyl,

Q is cyano, halo, nitro, OH, —CR a ═CR b R c , —C(O)NR d R e , carbonyl(C 1 -C 12 )alkyl, substituted or unsubstituted C 6 -C 12 aryl, or a combination comprising at least one of the foregoing groups, wherein each R a , R b , and R c are independently H or C 1 -C 18 alkyl, and wherein each R d and R e are independently H or C 1 -C 18 alkyl, carbonyl(C 1 -C 12 )alkyl,

x+y is an integer greater than two,

z is 0, 1, or 2, and

R is H, a substituted or unsubstituted C 1 -C 18 alkyl, a substituted or unsubstituted C 2 -C 18 alkenyl, a substituted or unsubstituted C 2 -C 18 alkynyl, a substituted or unsubstituted C 3 -C 18 cycloalkyl, a substituted or unsubstituted C 1 -C 18 haloalkyl, a substituted or unsubstituted C 2 -C 18 heterocycloalkyl, a substituted or unsubstituted C 6 -C 18 aryl, a substituted or unsubstituted C 7 -C 18 arylalkylene, or a substituted or unsubstituted C 3 -C 18 heteroaryl,

R′ is H or R′ together with R forms a substituted or unsubstituted C 2 -C 18 heterocycloalkyl, or substituted or unsubstituted C 2 -C 18 heteroaryl group, each having 5 to 8 ring members.

11. The copolymer of claim 10 , wherein R is H, methyl, ethyl, propyl, isopropyl, butyl, isobutyl, sec-butyl, methylthiomethylene, benzyl, indolylmethylene, or R and R′ together form propylene to provide a monomer having a 5-membered ring.

12. The copolymer of claim 10 , wherein Q is carbonyl(C 1 -C 12 )alkyl, substituted or unsubstituted C 6 -C 12 aryl, or a combination comprising at least one of the foregoing groups.

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 24, 2016
From: MAHANTHAPPA, MAHESH; THOMAS, GLEN; LIPSCOMB, CORINNE
To: WISCONSIN ALUMNI RESEARCH FOUNDATION
Reel/Frame 038092/0787 →
CONFIRMATORY LICENSE Recorded Jul 9, 2014
From: WISCONSIN ALUMNI RESEARCH FOUNDATION
To: NATIONAL SCIENCE FOUNDATION
Reel/Frame 033282/0096 →
Continuity (3)
Continuation 13738303 · Jan 10, 2013
Provisional Application 61587958 · Jan 18, 2012
Related Publication 20140296462A1 · Oct 2, 2014