IP Library Granted Patent US 8,067,648
Granted Patent B2
US 8,067,648 · App. 12/161,974 · Granted Nov 29, 2011

Method for synthesizing radioactive ligand having

Assignee: National Institute of Radiological Sciences
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Quick Facts
Patent No.
US 8,067,648
App. No.
12/161,974
Granted
Nov 29, 2011
Kind
B2
Abstract

A phenyl tin compound is synthesized by using a derivative having various functional groups and a bromo- or iodo-benzene ring as a labeling material of a radioactive ligand. On the other hand, a novel hydroxytosyl iodobenzene compound having an electron-donating group is obtained by oxidizing iodobenzene having one or more electron-donating groups and reacting it with tosylic acid. Then, a diphenyliodonium salt which is a labeling precursor is synthesized by reacting the resulting compound with various phenyl tin compounds. Finally, a 18 F-labeled ligand having various functional groups and a [ 18 F] fluorobenzene ring is synthesized by reacting the resulting diphenyliodonium salt with [ 18 F]F − .

Claims (48)

1. A method for synthesizing a radioactive ligand having a 18 F-labeled fluorobenzene ring of general formula (7),

comprising the steps of:

(A) reacting a phenylhalide compound of general formula (1)

wherein X is Br or I; R 1 , R 2 , R 3 , R 4 and R 5 may be the same or different and each represent a hydrogen atom, an alkyl group or a heteroatom-containing functional group, provided that all of R 1 , R 2 , R 3 , R 4 and R 5 are not a hydrogen atom or an alkyl group,

with a trialkyltin of general formula (2)

Sn(R 10 ) 3   ( 2 )

wherein R 10 represents an alkyl group

in the presence of a palladium catalyst to obtain a phenyltin compound of general formula

wherein X, R 1 , R 2 , R 3 , R 4 , R 5 and R 10 are as defined above;

(B) oxidizing an iodobenzene compound of general formula (4)

wherein E represents a functional group which donates electron to a π electron system, and n is 1, 2, 3, 4 or 5,

and then reacting the oxidized compound with toluenesulfonic acid monohydrate to obtain a hydroxytosyliodobenzene compound of general formula (5)

wherein Ts represents a toluenesulfonyl group; and E and n are as defined above;

(C) reacting the hydroxytosyliodobenzene compound of general formula (5) with the phenyltin compound of general formula (3) to obtain a diphenyliodonium salt of general formula (6)

wherein R 1 , R 2 , R 3 , R 4 , R 5 , E, n and Ts are as defined above;

and

(D) reacting the diphenyliodonium salt of general formula (6) with [ 18 F]F − to obtain a radioactive ligand having a 18 F-labeled fluorobenzene ring of general formula (7)

wherein R 1 , R 2 , R 3 , R 4 and R 5 are as defined above.

2. A method for obtaining a hydroxytosyliodobenzene compound of general formula (5)

wherein Ts represents a toluenesulfonyl group; and E and n are as defined below,

by oxidizing an iodobenzene compound of general formula (4)

wherein E represents a functional group which donates electron to a π electron system, and n is 1, 2, 3, 4 or 5,

and then reacting the oxidized compound with toluenesulfonic acid monohydrate.

3. The method for synthesizing a radioactive ligand as claimed in claim 1 ,

wherein R 2 is —NR 6 (C═O)R 7 , R 6 is a 2,5-dimethoxybenzyl group, R 7 is a methyl group, R 3 is a phenoxy group, and R 1 , R 4 and R 5 are each a hydrogen atom.

4. The method for synthesizing a radioactive ligand as claimed in claim 1 ,

wherein R 1 is —CH 2 CH(NHR)COOR, R 3 and R 4 are —OR or —OCOR, R is a C 1-6 alkyl group, and R 2 and R 5 are each a hydrogen atom.

5. The method for synthesizing a radioactive ligand as claimed in claim 4 ,

wherein R is selected from the group consisting of methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl, tert-butyl, pentyl and hexyl group.

6. The method for synthesizing a radioactive ligand as claimed in claim 1 ,

wherein E is selected from the group consisting of —NR 2 , —OR, —NHCOR, —NHSO 2 R, —OCOR, —SR, and —R, wherein R is a hydrogen atom or a C 1-6 alkyl group.

7. The method for synthesizing a radioactive ligand as claimed in claim 2 ,

wherein E is selected from the group consisting of —NR 2 , —OR, —NHCOR, —NHSO 2 R, —OCOR, —SR, and —R, wherein R is a hydrogen atom or a C 1-6 alkyl group.

8. The method for synthesizing a radioactive ligand as claimed in claim 1 ,

wherein when n is 2, 3, 4 or 5, n quantities of E may be the same or different.

9. The method for synthesizing a radioactive ligand as claimed in claim 2 ,

wherein when n is 2, 3, 4 or 5, n quantities of E may be the same or different.

10. The method for synthesizing a radioactive ligand as claimed in claim 1 ,

wherein n=1, and 1 quantity of E is a methoxy group and is substituted at the para-position, relative to I of the benzene ring.

11. The method for synthesizing a radioactive ligand as claimed in claim 2 ,

wherein n=1, and 1 quantity of E is a methoxy group and is substituted at the para-position, relative to I of the benzene ring.

12. The method for synthesizing a radioactive ligand as claimed in claim 8 ,

wherein n=2, and 2 quantities of E are both a methoxy group and are substituted at the meta- and para-positions, relative to I of the benzene ring.

13. The method for synthesizing a radioactive ligand as claimed in claim 9 ,

wherein n=2, and 2 quantities of E are both a methoxy group and are substituted at the meta- and para-positions, relative to I of the benzene ring.

14. The method for synthesizing a radioactive ligand as claimed in claim 1 ,

wherein in step (B) the oxidized compound is a periodine compound, and wherein the iodobenzene compound of general formula (4)

is oxidized by reacting with peracetic acid or sodium borate in acetic acid to form the periodine compound.

Assignments (2)
CHANGE OF NAME Recorded Dec 12, 2018
From: NATIONAL INSTITUTE OF RADIOLOGICAL SCIENCES
To: NATIONAL INSTITUTES FOR QUANTUM AND RADIOLOGICAL SCIENCE AND TECHNOLOGY
Reel/Frame 048999/0314 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 24, 2008
From: SUZUKI, KAZUTOSHI; ZHANG, MING-RONG; KUMATA, KATSUSHI
To: NATIONAL INSTITUTE OF RADIOLOGICAL SCIENCES
Reel/Frame 021284/0268 →
Priority Claims (1)
JP 2006-021967 · Jan 31, 2006 · national
Continuity (1)
Related Publication 20090069592A1 · Mar 12, 2009