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Gavestinel sodium, GV-150526A

4,6-二氯-3-[(1e)-3-氧代-3-(苯氨基)-1-丙基]-1h-吲哚-2-羧酸钠Chemical Name: 4,6-Dichloro-3-[2(E)-(N-phenylcarbamoyl)vinyl]-1H-indole-2-carboxylic acid sodium salt
CAS No. 153436-22-7 (free acid)
项目整合开发状态: Phase III
项目研究机构: GlaxoSmithKline (Originator)
合成路线:GW150526 was easily prepared starting from the known 3-unsubstituted indole derivative (IV) following the general synthetic route described in Scheme 20235901a.The known indole derivative (IV) was formylated at the C-3 position according to the well known Vilsmaier-Haack procedure obtaining the intermediate (VI) in high yield.The subsequent Wittig-type olefination reaction afforded the compound (VII) with high regio control in the formation of the olefinic moiety.The hydrolysis of the ethyl ester group afforded GV-150526 as sodium salt derivative.
📌 参考资料/链接:
参考文献标题:3-(2-Carboxyindol-3-yl)propionic acid derivatives: Antagonists of the strychnine-insensitive glycine receptor associated with the N-methyl-D-aspartate receptor complex
文献作者:Salituro,F.G.; et al.
参考来源:J Med Chem 1990,33(11),2946-8

📄 详细内容


合成路线:GW150526 was easily prepared starting from the known 3-unsubstituted indole derivative (IV) following the general synthetic route described in Scheme 20235901a.The known indole derivative (IV) was formylated at the C-3 position according to the well known Vilsmaier-Haack procedure obtaining the intermediate (VI) in high yield.The subsequent Wittig-type olefination reaction afforded the compound (VII) with high regio control in the formation of the olefinic moiety.The hydrolysis of the ethyl ester group afforded GV-150526 as sodium salt derivative.

合成路线:Alternatively,for the synthesis of analogues of GV-150526 substituted at the terminal phenyl ring belonging to the C-3 side chain as shown in Scheme 20235902a,compound (I) was transformed int the intermediate (III) in high yield.Following chemoselective deprotection of the tert-butyl ester group,the free carboxylic acid derivative (IV) was submitted to amidation reaction using different synthetic methods.In particular,the activation of the carboxy group through the formation of the corresponding 2-pyridyl thioester,generated in situ by the mild oxidation-reduction condensation reaction in the presence of 2,2'-dipyridyl disulfide and PPh3,was found to be highly efficient,also in the case of poor nucleophilic aromatic amines,affording the desired amide derivatives (VI) in high yield (either from the isolated 2-pyridyl thioester intermediate (V) or from the acid (IV) using a one pot procedure).Finally,target compounds were easily prepared by basic hydrolysis of the 2-carboxyethyl ester protecting group.

参考文献标题:Identification and pharmacological characterization of GV150526,a novel glycine antagonist as potent neuroprotective agent
文献作者:Di Fabio,R.; Cugola,A.; Donati,D.; Ferinai,A.; Gaviraghi,G.; Ratti,E.; Trist,D.G.; Reggiani,A.
参考来源:Drugs Fut 1998,23(1),61


合成路线:Alternatively,for the synthesis of analogues of GV-150526 substituted at the terminal phenyl ring belonging to the C-3 side chain as shown in Scheme 20235902a,compound (I) was transformed int the intermediate (III) in high yield.Following chemoselective deprotection of the tert-butyl ester group,the free carboxylic acid derivative (IV) was submitted to amidation reaction using different synthetic methods.In particular,the activation of the carboxy group through the formation of the corresponding 2-pyridyl thioester,generated in situ by the mild oxidation-reduction condensation reaction in the presence of 2,2'-dipyridyl disulfide and PPh3,was found to be highly efficient,also in the case of poor nucleophilic aromatic amines,affording the desired amide derivatives (VI) in high yield (either from the isolated 2-pyridyl thioester intermediate (V) or from the acid (IV) using a one pot procedure).Finally,target compounds were easily prepared by basic hydrolysis of the 2-carboxyethyl ester protecting group.

参考文献标题:
文献作者:Struys,M.M.R.F.; et al.
参考来源:Tetrahedron 1993,49(10),2239


合成路线:Alternatively,for the synthesis of analogues of GV-150526 substituted at the terminal phenyl ring belonging to the C-3 side chain as shown in Scheme 20235902a,compound (I) was transformed int the intermediate (III) in high yield.Following chemoselective deprotection of the tert-butyl ester group,the free carboxylic acid derivative (IV) was submitted to amidation reaction using different synthetic methods.In particular,the activation of the carboxy group through the formation of the corresponding 2-pyridyl thioester,generated in situ by the mild oxidation-reduction condensation reaction in the presence of 2,2'-dipyridyl disulfide and PPh3,was found to be highly efficient,also in the case of poor nucleophilic aromatic amines,affording the desired amide derivatives (VI) in high yield (either from the isolated 2-pyridyl thioester intermediate (V) or from the acid (IV) using a one pot procedure).Finally,target compounds were easily prepared by basic hydrolysis of the 2-carboxyethyl ester protecting group.
参考文献标题:
文献作者:Davison,S.C.; et al.
参考来源:VCH Publichers: Stuttgart 1989,147(4),972-6


产品链接: CAS No. 153436-22-7››