IP Library Granted Patent US 8,987,452
Granted Patent B2
US 8,987,452 · App. 13/848,477 · Granted Mar 24, 2015

Synthesis of thiohydantoins

Inventors: Ouathek Ouerfelli (Fort Lee, NJ); Anna Dilhas (Basel, CH); Guangbin Yang (Forest Hills, NY); Hong Zhao (Rego Park, NY)
Assignee: Sloan-Kettering Institute for Cancer Research
C07D401/04C07C209/36C07C213/08C07C253/00C07C253/30C07D213/61C07D213/64C07D213/72C07D213/74C07D213/84C07C2101/04
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Quick Facts
Patent No.
US 8,987,452
App. No.
13/848,477
Granted
Mar 24, 2015
Kind
B2
Abstract

A novel synthesis of the anti-androgen, A52, which has been found to be useful in the treatment of prostate cancer, is provided. A52 as well as structurally related analogs may be prepared via the inventive route. This new synthetic scheme may be used to prepare kilogram scale quantities of pure A52.

Claims (12)

1. A method of synthesizing a compound of formula:

the method comprising:

coupling a substituted pyridine of formula:

with a compound of formula:

in the presence of thiophosgene to provide an imidohydantoin intermediate; and

hydrolyzing the imidohydantoin intermediate under suitable acidic conditions to form a product of formula:

2. The method of claim 1 , wherein the step of coupling is performed in N,N-dimethylacetamide as the solvent.

3. The method of claim 1 , wherein the step of coupling is performed at approximately 60° C.

4. The method of claim 1 , wherein the step of coupling is performed with approximately 1 equivalent of the substituted pyridine of formula:

and approximately 1 equivalent of the compound of formula:

5. The method of claim 4 , wherein the step of coupling is performed with approximately 1 equivalent of thiophosgene.

6. The method of claim 1 , wherein the step of coupling comprises irradiating the reaction mixture with microwaves.

Assignments (2)
CONFIRMATORY LICENSE Recorded Nov 6, 2017
From: SLOAN-KETTERING INST CAN RESEARCH
To: NATIONAL INSTITUTES OF HEALTH (NIH), U.S. DEPT. OF HEALTH AND HUMAN SERVICES (DHHS), U.S. GOVERNMENT
Reel/Frame 044711/0832 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 22, 2013
From: OUERFELLI, OUATHEK; DILHAS, ANNA; YANG, GUANGBIN; ZHAO, HONG
To: SLOAN-KETTERING INSTITUTE FOR CANCER RESEARCH
Reel/Frame 030847/0650 →
Continuity (4)
Continuation 12450423
Provisional Application 60908280 · Mar 27, 2007
Provisional Application 60909195 · Mar 30, 2007
Related Publication 20130225821A1 · Aug 29, 2013