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EP0165630A2 Expired / Lapsed EP ⏱️ 0.0 years remaining

Method of preparing a chlorinated, brominated, radiobrominated, iodinated and/or radioiodinated, aromatic or heteroaromatic compound, as well as a kit for preparing a diagnostic composition on the basis of this compound

Assignee: Mallinckrodt Inc
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Filing: 1985-05-20
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Granted: —
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Expires: 2005-05-20
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Abstract

Abstract The invention relates to a method of preparing a chlorinated, brominated, radiobrominated, iodinated and/or radio-iodinated aromatic or heteroaromatic compound, in which the (hetero)aromatic nucleus optionally comprises one or more additional substituents, by reacting the corresponding halogenated or diazonium-substituted compound in the presence of a water-soluble acid and of copper ions as a catalyst with a likewise water-soluble chloride, bromide radiobromide, iodide or radio-iodide, in which the reaction is carried out in the presence of one or more reduction agents, which are stable in acid medium, in a quantity exceeding the quantity of catalyst. The invention also relates to a composition suitable for diagnostic examination and to a kit for the preparation thereof. The invention further relates to a method and an equipment for the preparation of said composition.

Inventors

  • 👤 John Mertens

Bibliographic Details

Application Number —
Jurisdiction EP
Data Source google_patents
Last Synchronized 2026-11-07 21:30
CPC Classifications
C; C07; C07C; C07C63/00; C07C63/68; C07C63/70; A; A61; A61K; A61K51/00; A61K51/02; A61K51/04; A61K51/12; A61K51/1282; A61M; A61M5/00; A61M5/178; A61M5/31; C07B; C07B39/00; C07C45/00; C07C45/61; C07C45/63; C07C51/00; C07C51/347; C07C51/363; C07C57/00; C07C57/52; C07C57/58; A61K2123/00; C07B2200/00; C07B2200/05

Claims Analysis

Total Claims: 23
Claim 1
Independent Claim 90 words
A method of preparing a chlorinated, brominated, radiobrominated, iodinated and/or radioiodinated aromatic or heteroaromatic compound, in which the (hetero)aromatic nucleus comprises optionally one or more additional substituents, by reacting the corresponding halogenated or diazonium-substituted compound in the presence of a water--soluble acid and of copper ions as a catalyst with a likewise water-soluble chloride, bromide, radiobromide, iodide or radioiodide, characterized in that the reaction is carried out in the presence of one or more reduction agents, which are stable in acid medium, in a quantity exceeding the quantity of catalyst.
Claim 2
Independent Claim 90 words
A method of preparing a chlorinated, brominated, radiobrominated, iodinated and/or radioiodinated aromatic or heteroaromatic compound, in which the (hetero)aromatic nucleus comprises optionally one or more additional substituents, by reacting the corresponding halogenated or diazonium-substituted compound in the presence of a water--soluble acid and of copper ions as a catalyst with a likewise water-soluble chloride, bromide, radiobromide, iodide or radioiodide, characterized in that the reaction is carried out in the presence of one or more reduction agents, which are stable in acid medium, in a quantity exceeding the quantity of catalyst.
Claim 3
Dependent Claim 113 words
A method as claimed in Claim 1 of preparing a brominated, radiobrominated, iodinated or radioiodinated aromatic or heteroaromatic compound, in which the (hetero)-aromatic nucleus is a benzene nucleus, a naphthalene nucleus, a pyridine nucleus, a pyrimidine nucleus, a quinoline nucleus or an indole nucleus which comprises one or more additional substituents, by reacting the corresponding halogenated or diazonium-substituted compound in the presence of a water-soluble, acid and of copper ions as a catalyst with a likewise water-soluble bromide, radiobromide, iodide or radioiodide, characterized in that the reaction is carried out in the presence of one or more reduction agents, which are stable in acid medium, in a quantity exceeding the quantity of catalyst.
Claim 4
Dependent Claim 85 words
A method as claimed in Claim 2 of preparing iodine--containing contrast media, for example iophendylate and other ones on the basis of 2-, 2,4- or 2,4,6-substituted 1,3,5-triiodobenzene, by reacting the corresponding brominated or diazonium-substituted compound in the presence of a water-soluble acid and of copper ions as a catalyst with a likewise water-soluble iodide, characterized in that the reaction is carried out in the presence of one or more reduction agents, which are stable in acid medium, in a quantity exceeding the quantity of catalyst.
Claim 5
Dependent Claim 98 words
A method as claimed in Claim 2 of preparing starting substances for radioiodinated diagnostics, which starting substances are selected from the group consisting of o-iodohippuric acid or salts thereof, iodoamphetamine or derivatives thereof, iodo-ω-phenyl fatty acids or salts thereof and rose bengal, by reacting the corresponding brominated or diazonium-substituted compound in the presence of a water-soluble acid and of copper ions as a catalyst with a likewise water-soluble iodide, characterized in that the reaction is carried out in the presence of one or more reduction agents, stable in acid medium, in a quantity exceeding the quantity of catalyst.
Claim 6
Dependent Claim 169 words
A method as claimed in Claim 2 of preparing radio- iodinated diagnostics selected from the group consisting of radioiodinated o-iodohippuric acid or salts thereof, iodoamphetamine or derivatives thereof, iodo-Ú-phenyl fatty acids or salts thereof, rose bengal, N-iodoquinolyl-N'--N'-dimethylpropanediamine, N,N,N'-trimethyl-N'-(2-hydroxy-3-methyl-5-iodobenzyl)-1,3-propanediamine, p-iodosulphonamide, N-iodophenylsulphonyl-N'-ethyl urea, gliben- clamide, 3-iodo-4-aminophenylethylamine, N,N-dimethyliodo- benzylamine, substituted or non-substituted iodopyridines or iodopyridineoxides, mono- and triiodobenzoic acid, N--[3-acetyl-4-(3-isopropylamino-2-hydroxy)propoxyphenyl]-iodobenzamide, iodinated indocyanine green, iodinated hy- droxybenzylpindolol, iodinated thiouracil, iodinated estradiol, halogenated phenothiazines, halogenated benzodiazepines, halogenated metyrapone, halogenated butyrophenone derivatives, halogenated dibenzazepines, halogenated thyroid gland hormones such as 3,3'-diiodothyrosine, 3,3',5--triiodothyrosine and 3,3',5,5'-tetraiodothyrosine, halogenated benzylguanidine, iodoantipyrine, and iodine-containing contrast media, for example iophendylate and other ones on the basis of 2-,2,4- or 2,4,6-substituted 1,3,5--triiodobenzene, by reacting the corresponding non-labelled bromine or iodine-substituted compound in the presence of a water-soluble acid and of copper ions as a catalyst with a likewise water-soluble radioactive iodide, characterized in that the reaction is carried out in the presence of one or more reduction agents, which are stable in acid medium, in a quantity exceeding the quantity of catalyst.
Claim 7
Dependent Claim 27 words
A method as claimed in Claim 5, characterized in t at sodium iodide or potassium iodide labelled with iodine-123 or iodine-131 is used as a radioactive iodide.
Claim 8
Independent Claim 52 words
A method as claimed in any of the preceding claims, chracterized in that an Sn(II) salt is used as a reduc- ticn agent whether or not in the presence of one or more antioxidants, preferably selected from the group consisting of metallic tin, ascorbic acid, citric acid, a monosaccharide or gentisic acid.
Claim 9
Independent Claim 33 words
A method as claimed in any of the Claims 1-6, characterized in that ascorbic acid, isoascorbic acid, citric acid, a monosaccharide, or a sulphite, preferably ascorbic acid, is used as a reduction agent.
Claim 10
Dependent Claim 75 words
A method as claimed in Claim 8 of preparing radio- iodinated o-iodohippuric acid or salts thereof, iodoam- phetamine or derivatives thereof, or iodo-ω-phenyl fatty acids or salts thereof, by reacting the corresponding non--adioactive bromine or iodine-substituted compound in the presence of a water-soluble acid and of copper ions as a catalyst with a likewise water-soluble radioactive iodide, characterized in that the reaction is carried out in the presence of ascorbic acid as a reduction agent.
Claim 11
Independent Claim 43 words
A method of preparing radioiodinated o-iodohippu- ric acid or salts thereof, by reacting the corresponding non-radioactive bromine or iodine-substituted compound with a water-soluble radioactive iodide, characterized in that the reaction is carried out in the presence of ascorbic acid as a reduction agent.
Claim 12
Independent Claim 43 words
A method of preparing radioiodinated o-iodohippu- ric acid or salts thereof, by reacting the corresponding non-radioactive bromine or iodine-substituted compound with a water-soluble radioactive iodide, characterized in that the reaction is carried out in the presence of ascorbic acid as a reduction agent.
Claim 13
Independent Claim 46 words
A method as claimed in any of the preceding Claims characterized in that the reaction is carried out in a aiqueous solution which optionally comprises salts and one or more water-miscible organic solvents, preferably in a solution which is entirely or substantially free from organic solvent.
Claim 14
Independent Claim 27 words
A method as claimed in any of the preceding Claims, characterized in that the reaction is carried out at a temperature of approximately 121°C, preferably approximately 100°C.
Claim 15
Dependent Claim 48 words
A composition suitable for diagnostic examination, which comprises, in addition to a pharmaceutically acceptable formulation liquid and/or one or more auxiliary substances, a iodine-containing contrast medium, characterized in that the composition comprises a contrast medium prepared according to any of the Claims 3, 7, 8, 11 and 12.
Claim 16
Dependent Claim 45 words
14, A composition, suitable for diagnostic examination, which comprises, in addition to a pharmaceutically acceptable formulation liquid and/or one or more auxiliary substances, a radioiodinated diagnostic, characterized in that the composition comprises a diagnostic prepared according to any of the Claims 1, 2 and 5-12.
Claim 17
Independent Claim 177 words
A method of preparing an injectable composition as claimed in Claims 13 or 14, characterized in that a pharmaceutically acceptable formulation liquid, which may comprise one or more auxiliary substances and is accomodated in at least one supply syringe, is added to the radioiodinated diagnostic, which radiodiagnostic containing substance is accomodated in a vial, sealingly closed with a pierceable stopper, said addition being carried out by piercing the stopper of said vial with the needle or needles of said supply syringe or syringes, and by then allowing the formulation liquid in said supply syringe or syringes to communicate with the atmospheric pressure to enable said liquid to reach the solution in the vial through the needle or needles, and that the composition in the vial thus obtained is then transferred to an injection syringe by piercing the stopper of said vial with the needle of said injection syringe and by then sucking the composition into the injection syringe, during which addition and/or transfer said formulation liquid and/or injectable composition preferably flow(s) through at least one sterilizing filter.
Claim 18
Dependent Claim 200 words
An equipment for carrying out the method as claimed in claim 15, characterized in that the equipment comprises (a) at least one supply syringe, provided with a cylindrical barrel for accomodating a formulation liquid, to which barrel a hollow needle is sealingly connected and in which barrel a plunger is movably positioned, the cylindrical side-wall of said barrel being provided with at least one aperture in such distance from the attached needle, that the formulation liquid to be accomodated in the barrel can be separated from the aperture in the barrel wall by means of the plunger, but that by withdrawing the plunger said aperture can allow said formulation liquid to communicate with the atmospheric pressure outside the syringe, (b) a vial for accomodating a radiodiagnostic containing subtance, which vial is sealingly closed with a pierceable stopper, and (c) an injection syringe, provided with a cylindrical barrel for accomodating an injectable composition, to which barrel a hollow needle is sealingly connected, if desired, through an intermediately positioned sterilizing filter means, the needle having a length sufficient for reaching the bottom of the vial after having pierced the stopper of said vial, and in which barrel a plunger is movably positioned.
Claim 19
Dependent Claim 107 words
A syringe for an equipment as claimed in Claim 16, provided with a cylindrical-barrel for accomodating a formulation liquid, to which barrel a hollow needle is sealingly connected and in which barrel a plunger is novably positioned, characterized in that the cylindrical side-wall of the barrel is provided with at least one aperture in such distance from the attached needle, that the formulation liquid to be accomodated in the barrel can be separated from the aperture in the barrel wall by means of the plunger, but that by withdrawing the plunger said aperture can allow said formulation liquid to communicate with the atmospheric pressure outside the syringe.
Claim 20
Dependent Claim 95 words
A kit for preparing a composition suitable for radiodiagnostic examination, comprising a bromine- or iodine-substituted aromatic or heteroaromatic compound, in which the (hetero)aromatic nucleus optionally comprises one or more additional substituents, a water-soluble acid, a copper salt and optionally a pharmaceutically acceptable formulation liquid and/or auxiliary substances, characterized in that the kit comprises in addition one or more reduction agents, which are stable in acid medium, and instructions for use stipulating that the radioactive diagnostic can be prepared by using the method as claimed in any of the Claims 1, 2, 5-9, 11 and 12.
Claim 21
Dependent Claim 28 words
A kit as claimed in Claim 18, characterized in that the kit comprises as a iodine-containing compound one of the compounds as claimed in Claim 3 or 4.
Claim 22
Dependent Claim 29 words
A kit as claimed in Claim 18 or 19, characterized in that the kit comprises as a reduction agent a reduction agent as claimed in Claim 7 or 8.
Claim 23
Dependent Claim 61 words
A kit for preparing a composition suitable for radiodiagnostic examination, comprising o-iodohippuric acid or a salt thereof, and optionally a pharmaceutically acceptable formulation liquid and/or auxiliary substances, characterized in that the kit moreover comprises ascorbic acid as a reduction agent and instructions for use stipulating that the radioactive diagnostic can be prepared by using the method as claimed in Claim 10.

References Cited (Backward Citations)

EP0011858A1 Cited
US4298591A Cited

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