IP Library Granted Patent US 9,895,454
Granted Patent B2
US 9,895,454 · App. 15/323,046 · Granted Feb 20, 2018

Metal oxide catalyzed radiofluorination

Inventors: Maxim Sergeev (Los Angeles, CA); Federica Morgia (Los Angeles, CA); Robert Michael Van Dam (Los Angeles, CA); Mark Lazari (North Hills, CA)
Assignee: THE REGENTS OF THE UNIVERSITY OF CALIFORNIA
A61K51/04A61K51/0446A61K51/0453A61K51/0455A61K51/0459A61K51/0491B01J21/063C07B59/001C07B59/002C07B59/005C07C17/361C07C67/333C07C201/12C07C253/30C07D207/09C07D207/16C07D213/61C07D217/22C07D241/16C07D405/06C07H19/052C07B2200/05C07C2101/14
View Patent ↗
Loading inventors, assignments & file history…
Monitor This Case
Get email alerts when status or documents change.
Order Certified Copies
Most orders are placed with the USPTO same day — all within 24 business hours.
Order via The Patent Place →
Pre-filled with this patent's details
Quick Facts
Patent No.
US 9,895,454
App. No.
15/323,046
Granted
Feb 20, 2018
Kind
B2
Abstract

Inter alia, the first titania-catalyzed [ 18 F]-radiofluorination in highly aqueous medium is provided. In embodiments, the method utilizes titanium dioxide, 1:1 acetonitrile-thexyl alcohol solvent mixture and tetrabutylammonium bicarbonate as a base. Radiolabeling may be directly performed with aqueous [ 18 F]fluoride without the need for drying/azeotroping step, which reduces radiosynthesis time while keeping high fluoride conversion. The general applicability of the synthetic strategy to the synthesis of the wide range of PET probes from tosylated precursors is demonstrated.

Claims (19)

1. A method of forming an [ 18 F]-labeled organic compound in an aqueous medium, the method comprising:

combining within an aqueous medium an aqueous [ 18 F] fluoride, a transition metal oxide and an organic compound precursor comprising a reactive carbon; and

allowing said aqueous [ 18 F] fluoride source to react with said reactive carbon thereby forming said [ 18 F]-labeled organic compound,

wherein said transition metal oxide is chromium(VI) oxide, molybdenum(VI) oxide, platinum(IV) oxide, rhenium(VI) oxide, rhenium(VII) oxide, ruthenium(IV) oxide, tantalum(V) oxide, tin(IV) oxide, vanadium(IV) oxide, vanadium(V) oxide, yttrium(III) oxide, zirconium(IV) oxide, chromium(III) oxide, bismuth(III) oxide, manganese(IV) oxide, tungsten(IV) oxide, molybdenum(IV) oxide, tungsten(VI) oxide, palladium(II) oxide, iron(II) oxide, zinc(II) oxide, indium(III) oxide, copper(II) oxide, niobium(IV) oxide, niobium(V) oxide, or titanium(IV) oxide.

2. The method of claim 1 , wherein said organic compound precursor is an aryl organic compound precursor and said [ 18 F]-labeled organic compound is an [ 18 F]-labeled aryl organic compound.

3. The method of claim 1 , wherein said aqueous medium is less than about 5%, 10%, 15%, 20% or 25% water.

4. The method of claim 1 , wherein said [ 18 F]-labeled organic compound is a positron emission tomography probe.

5. The method of claim 1 , wherein said reacting is SN2 nucleophilic substitution reacting.

6. The method of claim 1 , wherein the reactive carbon forms part of a substituted or unsubstituted aryl, substituted or unsubstituted heteroaryl, substituted or unsubstituted alkyl, substituted or unsubstituted heteroalkyl, substituted or unsubstituted cycloalkyl or substituted or unsubstituted heterocycloalkyl.

7. The method of claim 1 , wherein the reactive carbon forms part of a substituted or unsubstituted alkyl, substituted or unsubstituted heteroalkyl, substituted or unsubstituted cycloalkyl or substituted or unsubstituted heterocycloalkyl.

8. The method of claim 1 , wherein said transition metal oxide is palladium(II) oxide, iron(II) oxide, zinc(II) oxide, indium(III) oxide, copper(II) oxide, niobium(IV) oxide, niobium(V) oxide, or titanium(IV) oxide.

9. The method of claim 1 , wherein said transition metal oxide is TiO 2 , NbO 2 , Nb 2 O 5 , In 2 O 3 , or CuO.

10. The method of claim 1 , wherein said aqueous medium further comprises a base.

11. The method of claim 1 , wherein said aqueous medium further comprises an ammonium base.

12. The method of claim 1 , wherein said aqueous medium further comprises an ammonium bicarbonate base.

13. The method of claim 1 , wherein said aqueous medium further comprises an alcohol co-solvent, optionally MeOH, EtOH, n-PrOH, i-PrOH, t-BuOH, tHexOH, n-octanol or cyclohexanol.

14. The method of claim 1 , wherein said aqueous medium further comprises an alcohol co-solvent, optionally t-BuOH, tHexOH, n-octanol or cyclohexanol.

15. The method of claim 1 , wherein said organic compound precursor is attached to a tosylate, benzenesulfonyl, 4-nitrobenzenesulfonyl, methanesulfonyl, ethanesulfonyl, trifluoromethylsulfonyl, or 1,1,2,2,2-pentafluoroethane-1-sulfonyl moiety.

16. The method of claim 1 , wherein said aqueous [ 18 F] fluoride is generated from a cyclotron and is not dried or azeotroped after generation from said cyclotron.

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 25, 2017
From: SERGEEV, MAXIM; MORGIA, FEDERICA; VAN DAM, ROBERT MICHAEL; LAZARI, MARK
To: THE REGENTS OF THE UNIVERSITY OF CALIFORNIA
Reel/Frame 043407/0405 →
CONFIRMATORY LICENSE Recorded Jan 31, 2017
From: UNIVERSITY OF CALIFORNIA LOS ANGELES
To: NATIONAL INSTITUTES OF HEALTH (NIH), U.S. DEPT. OF HEALTH AND HUMAN SERVICES (DHHS), U.S. GOVERNMENT
Reel/Frame 041566/0370 →
Continuity (2)
Provisional Application 62020840 · Jul 3, 2014
Related Publication 20170224851A1 · Aug 10, 2017