IP Library Granted Patent US 10,189,803
Granted Patent B2
US 10,189,803 · App. 15/270,651 · Granted Jan 29, 2019

Synthesis of therapeutic and diagnostic drugs centered on regioselective and stereoselective ring opening of aziridinium ions

Inventor: Hyun-Soon Chong (Chicago, IL)
Assignee: ILLINOIS INSTITUTE OF TECHNOLOGY
C07D295/15C07B43/00C07B53/00C07C209/08C07C209/10C07C209/62C07C209/74C07C213/00C07C227/16C07C227/18C07C247/10C07C253/14C07C319/04C07C319/14C07C327/06C07C327/30C07C331/28C07D207/404C07D207/408C07D209/16C07D209/48C07D217/04C07D221/06C07D221/10C07D233/61C07D255/02C07D265/32C07D271/12C07J43/003C07B2200/07C07C2601/14C07C2602/08
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Quick Facts
Patent No.
US 10,189,803
App. No.
15/270,651
Granted
Jan 29, 2019
Kind
B2
Abstract

Stereoselective and regioselective synthesis of compounds via nucleophilic ring opening reactions of aziridinium ions for use in stereoselective and regioselective synthesis of therapeutic and diagnostic compounds.

Claims (48)

1. A method of stereoselective or regioselective synthesis through ring opening of aziridinium ions, comprising:

converting a substituted β amino alcohol to a substituted alkylating agent;

converting the substituted alkylating agent in the presence of halosequestering agent selected from AgClO 4 , AgOTf, Ag 2 CO 3 , AgOTs, AgNO 3 , AgSbF 6 , or AgBF 4 to a substituted aziridinium ion selected from:

where: Y is a halide or a non-nucleophilic counter anion selected from perchlorate or tetrafluoroborate; each of R 1-4 independently is hydrogen, carboxyalkyl, alkylamido, alkyl, allyl, benzyl, benzyloxyalkyl, cycloalkyl, heterocyclyl, alkoxy, aryl, CH 2 Ar, aryloxy, hydroxyaryl, heteroaryl, phenyl, vinyl, alkynyl, alkenyl, substituted carbonyl, halo, haloalkyl, nitrile, oxo, substituted oxo, substituted silyl, thiol, benzhydryl, silyl, substituted carboxyl, hydroxyalkyl, aminoalkyl, alkoxycarbonyl, alkylamido, furannylalkyl, alkylthioalkyl, arylhydroxyalkyl, indanyl, indolylalkyl, naphthylalkyl, imidazolylalkyl, pyridylalkyl, phthalimidyl, maleimidyl, benzothiophenylalkyl, thiophenylalkyl, thioalkyl, thioaryl, thiobenzyl, hydroxy, tosyl, nosyl, a protected amine, carboxyl, carboxyalkyloxy, amino, carboxylic acid, haloalkylamido, aldehyde, alkylamino, amido, trityl, tert-butyloxycarbonyl, carbobenzyloxy, acetyl dimethoxybenzyl, p-methoxybenzyl, any two vicinal carbons of R 1 and R 2 together form a fused ring, any two geminal carbons, R 1 and R 2 are bonded together and form a spiro ring, any of R 1-4 is attached to chiral carbon, or is one of:

where n=1-10 and X is hydrogen, halo, cyano, alkyl, aryl, hydroxyl, nitro, amino, alkylamino, dialkylamino, substituted amine, substituted carbonyl, isocyanate, cyanate ester, protected amine, protected hydroxyl, protected carboxyl, boronic acid, borinic acid, borinate ester, triflate, silyl, substituted silyl, thiocyano, isothiocyano, alkoxy, aryloxy, carboxyl, carboxylic acid, carboxyalkyl, carboxyalkyloxy, ester, amido, aldehydo, alkylamido, haloalkylamido, and R 3-4 can also be:

where: n=1-3; Ar is an aromatic ring bonded to one of the n carbons; R 5 is as defined for R 1 -R 4 ; and R′ independently is OH, NH 2 , NR″ 2 , or OR″, wherein R″ independently is alkyl, tert-butyl, allyl, benzyl, CH 2 Ar, silyl, trityl, an amine protecting group, a carboxyl protecting group, or a hydroxyl protecting group, and Ar in CH 2 Ar represents an aromatic ring; and

stereoselectively or regioselectively reacting the aziridinium ion in situ with a nucleophile in a nucleophilic ring opening reaction to obtain a compound.

2. The method of claim 1 , wherein the substituted alkylating agent is a substituted β-amino halide comprising:

3. The method of claim 1 , further comprising stereoselectively or regioselectively reacting the aziridinium ion with an aromatic compound including:

where X is defined as above; Y is NH, O, or S.

4. The method of claim 3 , wherein the compound is tryptamine.

5. The method of claim 1 , further comprising stereoselectively or regioselectively reacting the aziridinium ion with an organometallic compound or a reducing agent comprising hydride.

6. The method of claim 5 , wherein the compound comprises a chiral alpha amine.

7. The method of claim 1 , further comprising stereoselectively or regioselectively reacting the aziridinium ion with a dialkyl malonic ester.

8. The method of claim 1 , wherein the stereoselective or regioselective reaction of the aziridinium ion is an intramolecular nucleophilic reaction in the presence of a catalyst.

9. The method of claim 1 , wherein the synthesis occurs without isolation of any intermediate compound.

10. A method of stereoselective or regioselective synthesis through ring opening of aziridinium ions, comprising:

converting a substituted β amino alcohol to a substituted aziridinium ion selected from:

where: Y is a halide or a non-nucleophilic counter anion selected from perchlorate or tetrafluoroborate; each of R 1-4 independently is hydrogen, carboxyalkyl, alkylamido, alkyl, allyl, benzyl, benzyloxyalkyl, cycloalkyl, heterocyclyl, alkoxy, aryl, CH 2 Ar, aryloxy, hydroxyaryl, heteroaryl, phenyl, vinyl, alkynyl, alkenyl, substituted carbonyl, halo, haloalkyl, nitrile, oxo, substituted oxo, substituted silyl, thiol, benzhydryl, silyl, substituted carboxyl, hydroxyalkyl, aminoalkyl, alkoxycarbonyl, alkylamido, furannylalkyl, alkylthioalkyl, arylhydroxyalkyl, indanyl, indolylalkyl, naphthylalkyl, imidazolylalkyl pyridylalkyl, phthalimidyl, maleimidyl, benzothiophenylalkyl, thiophenylalkyl, thioalkyl, thioaryl, thiobenzyl, hydroxy, tosyl, nosyl, a protected amine, carboxyl, carboxyalkyloxy, amino, carboxylic acid, haloalkylamido, aldehyde, alkylamino, amido, trityl, tert-butyloxycarbonyl, carbobenzyloxy, acetyl, dimethoxybenzyl, p-methoxybenzyl, any two vicinal carbons of R 1 and R 2 together form a fused ring, any two geminal carbons, R 1 and R 2 are bonded together and form a spiro ring, any of R 1-4 is attached to chiral carbon, or is one of:

where n=1-10 and X is hydrogen, halo, cyano, alkyl, aryl, hydroxyl, nitro, amino, alkylamino, dialkylamino, substituted amine, substituted carbonyl, isocyanate, cyanate ester, protected amine, protected hydroxyl, protected carboxyl, boronic acid, borinic acid, borinate ester, triflate, silyl, substituted silyl, thiocyano, isothiocyano, alkoxy, aryloxy, carboxyl, carboxylic acid, carboxyalkyl, carboxyalkyloxy, ester, amido, aldehydo, alkylamido, haloalkylamido, and R 3-4 can also be:

where: n=1-3; Ar is an aromatic ring bonded to one of the n carbons; R 5 is as defined for R 1 -R 4 ; and R′ independently is OH, NH 2 , NR″ 2 , or OR″, wherein R″ independently is alkyl, tert-butyl, allyl, benzyl, CH 2 Ar, silyl, trityl, an amine protecting group, a carboxyl protecting group, or a hydroxyl protecting group, and Ar in CH 2 Ar represents an aromatic ring; and

stereoselectively or regioselectively reacting the aziridinium ion in a nucleophilic ring opening reaction with a nucleophile selected from:

where m is 0 or 1 and R′ independently is OH, NH 2 , NR 2 ″, or OR″, wherein R″ independently is alkyl, tert-butyl, allyl, benzyl, CH 2 Ar, silyl, trityl, an amine protecting group, a carboxyl protecting group, or a hydroxyl protecting group, and each of R 7-9 are as defined above for R 1-5 ; any two vicinal carbons of R 7-9 together form a fused ring; any of R 7-9 is or is attached to chiral carbon; or one of:

where X is as defined above, to obtain a compound.

11. The method of claim 10 , further comprising:

converting a substituted β amino alcohol to a substituted alkylating agent;

converting the substituted alkylating agent to the substituted aziridinium ion; and

stereoselectively or regioselectively reacting the aziridinium ion with a nucleophile to obtain the compound.

12. The method of claim 11 , further comprising:

converting the substituted alkylating agent to the aziridinium ion in the presence of halosequestering agent selected from AgClO 4 , AgOTf, Ag 2 CO 3 , AgOTs, AgNO 3 , AgSbF 6 , or AgBF 4 ; and

stereoselectively or regioselectively reacting the aziridinium ion in situ with a nucleophile to obtain the compound.

13. The method of claim 10 , wherein the compound is one of:

14. The method of claim 13 , further comprising removing a protecting group selected from an amino, a carboxyl, or a hydroxyl protecting group from the compound using a deprotection reaction.

15. The method of claim 14 , further comprising converting a nitro group in the compound to an amino group.

16. The method of claim 15 , further comprising converting an amino group to an isothiocyanate group.

17. The method of claim 10 , further comprising:

converting the substituted alkylating agent to the aziridinium ion in the presence of halosequestering agent selected from AgClO 4 , AgOTf, Ag 2 CO 3 , AgOTs, AgNO 3 , AgSbF 6 , or AgBF 4 ; and

stereoselectively or regioselectively reacting the aziridinium ion in situ with the nucleophile in the presence of a base to obtain the compound.

18. The method of claim 10 , further comprising:

converting a substituted β amino alcohol to a substituted alkylating agent;

converting the substituted alkylating agent to the substituted aziridinium ion; and

stereoselectively or regioselectively reacting the aziridinium ion with a nucleophile to obtain the compound, wherein the reaction occurs without isolation of any intermediate compound.

19. A method of stereoselective or regioselective synthesis through ring opening of aziridinium ions, comprising:

converting a substituted β amino alcohol to a substituted alkylating agent;

converting the substituted alkylating agent to a substituted aziridinium ion in the presence of halosequestering agent selected from AgClO 4 , AgOTf, Ag 2 CO 3 , AgOTs, AgNO 3 , AgSbF 6 , or AgBF 4 ; and

stereoselectively or regioselectively reacting the aziridinium ion in situ with a nucleophile in a nucleophilic ring opening reaction to obtain a compound, wherein the synthesis occurs without isolation of any intermediate compound.

20. The method of claim 19 , wherein the aziridinium ion is:

where: Y is a halide, a perchlorate, or tetrafluoroborate, each of R 1-2 , independently is hydrogen, carboxyalkyl, alkylamido, alkyl, allyl, benzyl, benzyloxyalkyl, cycloalkyl, alkoxy, hydroxyalkyl, aryl, aryloxy, hydroxyaryl, heteroaryl, phenyl, vinyl, alkynyl, alkenyl, furannylalkyl, alkylthioalkyl, arylhydroxyalkyl, indanyl, indolylalkyl, naphthylalkyl , imidazolylalkyl, pyridylalkyl, benzothiophenylalkyl, thiophenylalkyl , thioalkyl, thioaryl, thiobenzyl, carboxyl, carboxyalkyloxy, aldehyde, ester, amido, or a protecting group, and each of R 3-4 independently comprises a tert-butyl group or a benzyl group.

Assignments (4)
CORRECTIVE ASSIGNMENT TO CORRECT THE ASSIGNEE NAME PREVIOUSLY RECORDED AT REEL: 70348 FRAME: 680. ASSIGNOR(S) HEREBY CONFIRMS THE ASSIGNMENT. Recorded Feb 28, 2025
From: ILLINOIS INSTITUTE OF TECHNOLOGY
To: CHONG, HYUN-SOON, PHD
Reel/Frame 070764/0706 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 27, 2025
From: ILLINOIS INSTITUTE OF TECHNOLOGY
To: CHONG, HYUN-SOON L, PHD.
Reel/Frame 070348/0680 →
CONFIRMATORY LICENSE Recorded Mar 2, 2018
From: ILLINOIS INSTITUTE OF TECHNOLOGY
To: NATIONAL INSTITUTES OF HEALTH (NIH), U.S. DEPT. OF HEALTH AND HUMAN SERVICES (DHHS), U.S. GOVERNMENT
Reel/Frame 045488/0090 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 23, 2016
From: CHONG, HYUN-SOON
To: ILLINOIS INSTITUTE OF TECHNOLOGY
Reel/Frame 040704/0641 →
Continuity (7)
Continuation In Part 14834516 · Aug 25, 2015
Continuation In Part 13896524 · May 17, 2013
Continuation In Part 12806754 · Aug 20, 2010
Continuation In Part PCTUS2009034902 · Feb 23, 2009
Provisional Application 61649437 · May 21, 2012
Provisional Application 61066636 · Feb 22, 2008
Related Publication 20170008863A1 · Jan 12, 2017
Cited By (3)
US 12,275,742 US 12,371,399 US 12,630,560