IP Library Granted Patent US 10,117,948
Granted Patent B2
US 10,117,948 · App. 15/187,169 · Granted Nov 6, 2018

Selective arylation of dichalcogenides in biomolecules

Inventors: Stephen L. Buchwald (Newton, MA); Bradley L. Pentelute (Cambridge, MA); Daniel T. Cohen (Brighton, MA); Chi Zhang (Cambridge, MA)
Assignee: Massachusetts Institute of Technology
A61K47/48246A61K38/14A61K47/64A61K47/6851C07K1/1075C07K1/1077C07K1/13C07K9/008C07K14/47
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Quick Facts
Patent No.
US 10,117,948
App. No.
15/187,169
Granted
Nov 6, 2018
Kind
B2
Abstract

Disclosed are chemical transformations for the conjugation of unprotected peptide biomolecules. The disclosed chemical transformations relate to methods of selective cysteine and selenocysteine functionalization of unprotected peptide and protein molecules. The processes feature several significant advantages over existing methods of peptide modification, including specificity towards selenocysteine over other nucleophiles (e.g., amines, hydroxyls), excellent functional group tolerance, and mild reaction conditions. Also disclosed are syntheses of arylated cysteine and arylated selenocysteine peptide compounds.

Claims (103)

1. A compound comprising

(a) substructure I:

wherein, independently for each occurrence,

A 1 is H, an amine protecting group, a natural or unnatural amino acid, a peptide, an oligopeptide, a polypeptide, or a protein;

A 5 is OH, —O(carboxylate protecting group), a natural or unnatural amino acid, a peptide, an oligopeptide, a polypeptide, or a protein;

 is a substituted phenyl radical selected from the group consisting of

x is 0, 1, 2, 3, 4, 5, or 6; and

R is H or alkyl; or

(b) substructure II:

wherein, independently for each occurrence,

A 1 is H, an amine protecting group, a natural or unnatural amino acid, a peptide, an oligopeptide, a polypeptide, or a protein;

A 5 is OH, —O(carboxylate protecting group), a natural or unnatural amino acid, a peptide, an oligopeptide, a polypeptide, or a protein;

 is a substituted phenyl radical selected from the group consisting of

x is 0, 1, 2, 3, 4, 5, or 6; and

R is H or alkyl.

2. A method

(a) according to Scheme 1:

wherein, independently for each occurrence,

A 1 is H, an amine protecting group, a natural or unnatural amino acid, a peptide, an oligopeptide, a polypeptide, or a protein;

A 5 is OH, —O(carboxylate protecting group), a natural or unnatural amino acid, a peptide, an oligopeptide, a polypeptide, or a protein;

 is a substituted phenyl radical selected from the group consisting of

 is a heteroaromatic moiety substituted with an electron withdrawing group;

x is 0, 1, 2, 3, 4, 5, or 6; and

R is H or alkyl;

(b) according to Scheme 2:

wherein, independently for each occurrence,

A 1 is H, an amine protecting group, a natural or unnatural amino acid, a peptide, an oligopeptide, a polypeptide, or a protein;

A 5 is OH, —O(carboxylate protecting group), a natural or unnatural amino acid, a peptide, an oligopeptide, a polypeptide, or a protein;

 is a substituted phenyl radical selected from the group consisting of

 is a heteroaromatic moiety substituted with an electron withdrawing group;

x is 0, 1, 2, 3, 4, 5, or 6; and

R is H or alkyl;

(c) according to Scheme 3:

wherein, independently for each occurrence,

A 1 is H, an amine protecting group, a natural or unnatural amino acid, a peptide, an oligopeptide, a polypeptide, or a protein;

A 2 , A 3 , and A 4 are selected from the group consisting of a natural amino acid, an unnatural amino acid, and a plurality of natural amino acids or unnatural amino acids;

A 5 is OH, —O(carboxylate protecting group), a natural or unnatural amino acid, a peptide, an oligopeptide, a polypeptide, or a protein;

 is a phenyl radical selected from the group consisting of

 is a substituted phenyl diradical selected from the group consisting of

 is a heteroaromatic moiety substituted with an electron withdrawing group;

x is 0, 1, 2, 3, 4, 5, or 6; and

R is H or alkyl;

(d) according to Scheme 4:

wherein, independently for each occurrence,

A 1 is H, an amine protecting group, a natural or unnatural amino acid, a peptide, an oligopeptide, a polypeptide, or a protein;

A 2 , A 3 , and A 4 are selected from the group consisting of a natural amino acid, an unnatural amino acid, and a plurality of natural amino acids or unnatural amino acids;

A 5 is OH, —O(carboxylate protecting group), a natural or unnatural amino acid, a peptide, an oligopeptide, a polypeptide, or a protein;

 is a phenyl radical selected from the group consisting of

 is a phenyl radical selected from the group consisting of

 is a heteroaromatic moiety substituted with an electron withdrawing group;

x is 0, 1, 2, 3, 4, 5, or 6; and

R is H or alkyl;

(e) according to Scheme 5:

wherein, independently for each occurrence,

A 1 is H, an amine protecting group, a natural or unnatural amino acid, a peptide, an oligopeptide, a polypeptide, or a protein;

A 5 is OH, —O(carboxylate protecting group), a natural or unnatural amino acid, a peptide, an oligopeptide, a polypeptide, or a protein;

 is a substituted phenyl radical selected from the group consisting of

 is a heteroaromatic moiety substituted with an electron withdrawing group;

x is 0, 1, 2, 3, 4, 5, or 6; and

R is H or alkyl;

(f) according to Scheme 6:

wherein, independently for each occurrence,

A 1 is H, an amine protecting group, a natural or unnatural amino acid, a peptide, an oligopeptide, a polypeptide, or a protein;

A 2 , A 3 , and A 4 are selected from the group consisting of a natural amino acid, an unnatural amino acid, and a plurality of natural amino acids or unnatural amino acids;

A 5 is OH, —O(carboxylate protecting group), a natural or unnatural amino acid, a peptide, an oligopeptide, a polypeptide, or a protein;

 is a phenyl radical selected from the group consisting of

 is a phenyl radical selected from the group consisting of

 is a heteroaromatic moiety substituted with an electron withdrawing group;

x is 0, 1, 2, 3, 4, 5, or 6; and

R is H or alkyl;

(g) according to Scheme 7:

wherein, independently for each occurrence,

A 1 is H, an amine protecting group, a natural or unnatural amino acid, a peptide, an oligopeptide, a polypeptide, or a protein;

A 2 , A 3 , and A 4 are selected from the group consisting of a natural amino acid, an unnatural amino acid, and a plurality of natural amino acids or unnatural amino acids;

A 5 is OH, —O(carboxylate protecting group), a natural or unnatural amino acid, a peptide, an oligopeptide, a polypeptide, or a protein;

 is a phenyl radical selected from the group consisting of

 is a substituted phenyl diradical selected from the group consisting of

 is a heteroaromatic moiety substituted with an electron withdrawing group;

x is 0, 1, 2, 3, 4, 5, or 6; and

R is H or alkyl; or

(h) according to Scheme 8:

wherein, independently for each occurrence,

A 1 is H, an amine protecting group, a natural or unnatural amino acid, a peptide, an oligopeptide, a polypeptide, or a protein;

A 2 , A 3 , and A 4 are selected from the group consisting of a natural amino acid, an unnatural amino acid, and a plurality of natural amino acids or unnatural amino acids;

A 5 is OH, —O(carboxylate protecting group), a natural or unnatural amino acid, a peptide, an oligopeptide, a polypeptide, or a protein;

 is a phenyl radical selected from the group consisting of

 is a phenyl radical selected from the group consisting of

 is a heteroaromatic moiety substituted with an electron withdrawing group;

x is 0, 1, 2, 3, 4, 5, or 6; and

R is H or alkyl.

3. A method of treating, killing or inhibiting the growth or proliferation of a bacterium, a fungus, a virus, or a parasite, comprising the step of:

contacting with the bacterium, fungus, virus, or parasite an effective amount of a compound of claim 1 , thereby treating killing or inhibiting the growth or proliferation of the bacterium, fungus, virus, or parasite.

4. A method of treating a disease in a subject in need thereof comprising the step of:

administering to the subject an effective amount of a compound of claim 1 , thereby treating the disease.

5. The compound of claim 1 comprising substructure I.

6. The compound of claim 1 , wherein

is a substituted phenyl radical selected from the group consisting of

7. The compound of claim 1 , wherein

is

8. The compound of claim 1 comprising substructure II.

9. The compound of claim 1 , wherein is a substituted phenyl radical selected from the group consisting of

10. The compound of claim 1 , wherein

is

Assignments (2)
CONFIRMATORY LICENSE Recorded Dec 20, 2017
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 044919/0698 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 14, 2016
From: BUCHWALD, STEPHEN L.; PENTELUTE, BRADLEY L.; COHEN, DANIEL T.; ZHANG, CHI
To: MASSACHUSETTS INSTITUTE OF TECHNOLOGY
Reel/Frame 039158/0826 →
Continuity (2)
Provisional Application 62182146 · Jun 19, 2015
Related Publication 20160367693A1 · Dec 22, 2016