IP Library › Granted Patent US 9,758,507
Granted Patent B2
US 9,758,507 · App. 14/967,871 · Granted Sep 12, 2017

Chiral synthesis of pyrrolidine core compounds en route to neuronal nitric oxide synthase inhibitors

Inventors: Richard B. Silverman (Winnetka, IL); Fengtian Xue (Baton Rouge, LA)
Assignee: Northwestern University
C07D401/06C07D401/12C07D493/08
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Quick Facts
Patent No.
US 9,758,507
App. No.
14/967,871
Granted
Sep 12, 2017
Kind
B2
Abstract

A chiral synthesis of pyrrolidine compounds en route to selective neuronal nitric oxide synthase inhibitors, and representative inhibitor compounds heretofore unattainable.

Claims (11)

1. A method of preparing a chiral (aminopyridinyl)alkyl-substituted pyrrolidine core compound, said method comprising:

providing a racemic di-N-Boc-protected 3,4-trans-(aminopyridinyl)alkyl-substituted pyrrolidine alcohol;

protecting said amino group of said (aminopyridinyl)alkyl-substituent with a Boc reagent, to provide a tri-Boc-protected pyrrolidine compound; and

resolving said racemic trans-alcohol by camphanic acid esterification, to provide separable cis-diastereorners.

2. The method of claim 1 wherein said pyrrolidine alcohol is substituted with a (4-methylpyridin-2-yl)methyl moiety.

3. The method of claim 1 wherein said pyrrolidine alcohol is protected with a silyl chloride reagent before said amino group protection.

4. The method of claim 3 wherein said alcohol protection is removed before said camphanic acid esterification.

5. The method of claim 1 comprising base hydrolysis of one said enantiomer of said racemate, to provide a chiral 4-hydroxypyrrolidine compound.

6. The method of claim 5 wherein said 4-hydroxypyrrolidine compound is allylated.

7. The method of claim 6 comprising oxidation of said allyl moiety of said chiral pyrrolidine compound to provide an aldehyde group, and reductive amination of said aldehyde group with an ethanamine.

8. The method of claim 1 comprising concurrent removal of three Boc-protecting groups.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 16, 2016
From: SILVERMAN, RICHARD B.; XUE, FENGTIAN
To: NORTHWESTERN UNIVERSITY
Reel/Frame 037739/0210 →
Continuity (4)
Division 14252478 · Apr 14, 2014
Division 13174982 · Jul 1, 2011
Provisional Application 61360727 · Jul 1, 2010
Related Publication 20160096821A1 · Apr 7, 2016