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Iofetamine hydrochloride I-123, Ro-23-1507/001, M-123, IMP, Spectamine A

(+-)-4-(碘-123I)-alpha-甲基-N-(1-甲基乙基)-苯乙胺 Chemical Name: (?-N-Isopropyl-p-[(123)I]-iodoamphetamine hydrochloride; (?-4-(Iodo-(123)I)-alpha-methyl-N-(1-methylethyl)benzeneethanamine hydrochloride; (?-p-Iodo-(123)I-N-isopropyl-alpha-methylphenethylamine hydrochloride
CAS No. 85068-76-4, 75917-92-9 (free base)
项目整合开发状态: Launched-1987
项目研究机构: Medi-Physics (Originator)
合成路线:1) Reductive amination of phenylacetone (I) with ammonium acetate and sodium cyanoborohydride (I) gives d,l-amphetamine (II),which is separated by distillation at reduced pressure from a secondary amine byproduct resulting from reaction of amphetamine with phenylacetone.Iodination of the N-acetyl-protected amine followed by acid hydrolysis yields a mixture of ortho-meta and para substituted iodoamphetamine,from which the para-isomer can be obtained by crystallization of the salt (IV) from hydrochloric acid.Reductive condensation of the primary amine salt with acetone and sodium cyanoborohydride then yields ofetamine (V).The free base is converted to the hydrochloride salt (VI) by treatment with dry HCl gas in ether.The acetate salt may be prepared by treatment of the free base with glacial acetic acid in ether,followed by addition of hexane or petroleum ether to precipitate the product.

合成路线:2) A route that does not involve controlled drugs (phenylacetone or amphetamine) proceeds from p-iodophenylacetic acid (VII).The starting material can be made in low yield by iodination of phenylacetic acid or by a two-step process from p-aminophenylacetic acid by diazotization and treatment with potassium iodide.Condensation of p-iodophenylacetic acid (VII) with acetic anhydride gives p-iodophenylacetone (VIII) in variable yields,depending on the purity of the starting carboxylic acid and en the choice of base.Reductive amination with isopropylamine then gives iofetamine (V) in good yield.

合成路线:3) A third sequence proceeds by condensation of p-iodobenzaldehyde (IX) with nitromethane,followed by reductive hydrolysis of the intermediate unsaturated nitrocompound,to yield p-iodophenylacetone (VIII).The final sequence is the same as in scheme 09034702a.
📌 参考资料/链接:
参考文献标题:Iofetamine (123I) hydrochloride
文献作者:Baldwin,R.M.
参考来源:Drugs Fut 1986,11(8),652

📄 详细内容


合成路线:3) A third sequence proceeds by condensation of p-iodobenzaldehyde (IX) with nitromethane,followed by reductive hydrolysis of the intermediate unsaturated nitrocompound,to yield p-iodophenylacetone (VIII).The final sequence is the same as in scheme 09034702a.

参考文献标题:Chemical and pharmacological aspects of cerebral cellular tracers
文献作者:Rapin,J.R.; Duterte,D.; le Poncin-Lafitte,M.; Coornaert,S.; Desplanches,G.; Bardy,A.; Askienazy,S.; Moretti,J.L.; Raynaud,C.
参考来源:Ann Radiol 1983,26(1),48


合成路线:2) A route that does not involve controlled drugs (phenylacetone or amphetamine) proceeds from p-iodophenylacetic acid (VII).The starting material can be made in low yield by iodination of phenylacetic acid or by a two-step process from p-aminophenylacetic acid by diazotization and treatment with potassium iodide.Condensation of p-iodophenylacetic acid (VII) with acetic anhydride gives p-iodophenylacetone (VIII) in variable yields,depending on the purity of the starting carboxylic acid and en the choice of base.Reductive amination with isopropylamine then gives iofetamine (V) in good yield.

参考文献标题:131I-labelled N-isopropyl-p-Iodoamphetamine
文献作者:Carlsen,L.; Andresen,K.
参考来源:Eur J Nucl Med 1982,7(6),280


合成路线:1) Reductive amination of phenylacetone (I) with ammonium acetate and sodium cyanoborohydride (I) gives d,l-amphetamine (II),which is separated by distillation at reduced pressure from a secondary amine byproduct resulting from reaction of amphetamine with phenylacetone.Iodination of the N-acetyl-protected amine followed by acid hydrolysis yields a mixture of ortho-meta and para substituted iodoamphetamine,from which the para-isomer can be obtained by crystallization of the salt (IV) from hydrochloric acid.Reductive condensation of the primary amine salt with acetone and sodium cyanoborohydride then yields ofetamine (V).The free base is converted to the hydrochloride salt (VI) by treatment with dry HCl gas in ether.The acetate salt may be prepared by treatment of the free base with glacial acetic acid in ether,followed by addition of hexane or petroleum ether to precipitate the product.

参考文献标题:Development of I-123 N-Isopropyl-p-iodoamphetamine: Exploration,synthesis,metabolism,toxicology,and radiation dosimetry
文献作者:Baldwin,R.M.; Lin,T.H.; Wu,J.L.
参考来源:16th Jpn Conf Rad Radioisotope (Dec 6-8,Tokio) 1983,45(23),77


合成路线:3) A third sequence proceeds by condensation of p-iodobenzaldehyde (IX) with nitromethane,followed by reductive hydrolysis of the intermediate unsaturated nitrocompound,to yield p-iodophenylacetone (VIII).The final sequence is the same as in scheme 09034702a.

参考文献标题:New ways of obtaining N-isopropyl-p-iodoamphetamine and pharmacokinetic studies in rat
文献作者:Rapin,J.R.; Bardy,A.; Coornaert,S.; et al.
参考来源:3rd Wordl Cong Nucl Med Biol (Aug,Paris) 1982,43598


合成路线:2) A route that does not involve controlled drugs (phenylacetone or amphetamine) proceeds from p-iodophenylacetic acid (VII).The starting material can be made in low yield by iodination of phenylacetic acid or by a two-step process from p-aminophenylacetic acid by diazotization and treatment with potassium iodide.Condensation of p-iodophenylacetic acid (VII) with acetic anhydride gives p-iodophenylacetone (VIII) in variable yields,depending on the purity of the starting carboxylic acid and en the choice of base.Reductive amination with isopropylamine then gives iofetamine (V) in good yield.

参考文献标题:Die Phenylbenzylbernsteinsaueren
文献作者:Stoermer,R.; Strioh,H.
参考来源:Chem Ver 1935,682112


合成路线:1) Reductive amination of phenylacetone (I) with ammonium acetate and sodium cyanoborohydride (I) gives d,l-amphetamine (II),which is separated by distillation at reduced pressure from a secondary amine byproduct resulting from reaction of amphetamine with phenylacetone.Iodination of the N-acetyl-protected amine followed by acid hydrolysis yields a mixture of ortho-meta and para substituted iodoamphetamine,from which the para-isomer can be obtained by crystallization of the salt (IV) from hydrochloric acid.Reductive condensation of the primary amine salt with acetone and sodium cyanoborohydride then yields ofetamine (V).The free base is converted to the hydrochloride salt (VI) by treatment with dry HCl gas in ether.The acetate salt may be prepared by treatment of the free base with glacial acetic acid in ether,followed by addition of hexane or petroleum ether to precipitate the product.

参考文献标题:1- Phenylethylaminderivative als optisch aktive Adsorbentien
文献作者:Donow,F.; Blanschke,G.
参考来源:Chem Ver 1975,1082792


产品链接: CAS No. 85068-76-4››

产品链接: CAS No.75917-92-9››