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Viramidine hydrochloride, Ribamidine hydrochloride, ICN-3142(hydrochloride), AVS-000206, AVS-206, Viramidine

三氮唑核苷脒盐酸盐 利巴韦林 Chemical Name: 1-beta-D-Ribofuranosyl-1,2,4-triazole-3-carboxamidine hydrochloride; 1-beta-D-Ribofuranosyl-1H-1,2,4-triazole-3-carboximidamide hydrochloride
CAS No. 40372-00-7, 119567-79-2 (free base)
项目整合开发状态: Phase III
项目研究机构: Valeant (Originator)
合成路线:The condensation of 1-O-acetyl-2,3,5-tri-O-benzoyl-beta-D-ribofuranose (X) with 1,2,4-triazole-3-carboxylic acid methyl ester (VII) by means of PNPP at 160 C C gives 1-(2,3,5-tri-O-benzoyl-beta-D-ribofuranosyl)-1,2,4-triazole-3-carboxylic acid methyl ester (XI),which is finally treated with NH4OH in methanol.

合成路线:The silylation of 1,2,4-triazole-3-carboxylic acid methyl ester (VII) with hexamethyldisylazane (HMDS) gives 1-(trimethylsilyl)-1,2,4-triazole-3-carboxylic acid methyl ester (XII),which is condensed with 2,3,5-tri-O-benzoyl-beta-D-ribofuranosyl bromide (XIII) by means of PNPP at 160 C to afford the previously described intermediate 1-(2,3,5-tri-O-benzoyl-beta-D-ribofuranosyl)-1,2,4-triazole-3-carboxylic acid methyl ester (XI).

合成路线:The condensation of 1,2,3,5-tetra-O-acetyl-beta-D-ribofuranose (XIV) with 1,2,4-triazole-3-carboxylic acid methyl ester (VII) by means of PNPP at 160 C gives 1-(2,3,5-tri-O-acetyl-beta-D-ribofuranosyl)-1,2,4-triazole-3-carboxylic acid methyl ester (XV),which is finally treated with NH4OH in methanol.The condensation of 2,3,5-tri-O-acetyl-beta-D-ribofuranosyl bromide (XVI) with 1-(trimethylsilyl)-1,2,4-triazole-3-carboxylic acid methyl ester (XII) in acetonitrile gives the previously reported intermediate 1-(2,3,5-tri-O-acetyl-beta-D-ribofuranosyl)-1,2,4-triazole-3-carboxylic acid methyl ester (XV).

合成路线:Viramidine can be synthesized by several related ways: 1) Reaction of triethyl orthoformate (I) with 1-cyanoformimidic acid hydrazide (II) by means of anhydrous HCl in dioxane gives 1,2,4-triazole-3-carbonitrile (III),which is condensed with tetra-O-acetyl-?D-ribofuranose (IV) by means of di-p-nitrophenyl phosphate (BNPP) at 150 oC to yield a mixture of the regioisomeric ribonucleosides (V) and (VI),easily separated by chromatography.Finally,the suitable regiosomer 3-cyano-1-(2,3,5-tri-O-acetyl-?D-ribofuranosyl)-1,2,4-triazole (V) is treated with anhydrous NH3 and NH4Cl at 85 oC in a pressure bomb (1,2).2) Alternatively,condensation of 2,3,5-tri-O-acetyl-?D-ribofuranosyl bromide (VII) with 1-(trimethylsilyl)-1,2,4-triazole-3-carbonitrile (VIII) - prepared by treatment of triazole (III) with hexamethyldisilazane in dry acetonitrile - in acetonitrile also gives the regioisomeric mixture of nucleosides (V) and (VI) (1).3) Acylation of ribavirin (1-?D-ribofuranosyl-1,2,4-triazole-3-carboxamide) (IX) with Ac2O and pyridine gives the triacetate (X),which is dehydrated by means of POCl3 and triethylamine in chloroform to yield 3-cyano-1-(2,3,5-tri-O-acetyl-?D-ribofuranosyl)-1,2,4-triazole (V).Treatment of nucleoside (V) with NaOMe in methanol affords the methyl carboximidate (XI),which is finally treated with NH4Cl and dry NH3 gas in methanol (3).
📌 参考资料/链接:
参考文献标题:1,2,4-Triazole nucleosides
文献作者:Laguna,N.; Robins,R.K.; Witkowski,J.T.(ICN Pharmaceuticals,Inc.)
参考来源:DE 2220246; US 3798209

📄 详细内容


合成路线:Viramidine can be synthesized by several related ways: 1) Reaction of triethyl orthoformate (I) with 1-cyanoformimidic acid hydrazide (II) by means of anhydrous HCl in dioxane gives 1,2,4-triazole-3-carbonitrile (III),which is condensed with tetra-O-acetyl-?D-ribofuranose (IV) by means of di-p-nitrophenyl phosphate (BNPP) at 150 oC to yield a mixture of the regioisomeric ribonucleosides (V) and (VI),easily separated by chromatography.Finally,the suitable regiosomer 3-cyano-1-(2,3,5-tri-O-acetyl-?D-ribofuranosyl)-1,2,4-triazole (V) is treated with anhydrous NH3 and NH4Cl at 85 oC in a pressure bomb (1,2).2) Alternatively,condensation of 2,3,5-tri-O-acetyl-?D-ribofuranosyl bromide (VII) with 1-(trimethylsilyl)-1,2,4-triazole-3-carbonitrile (VIII) - prepared by treatment of triazole (III) with hexamethyldisilazane in dry acetonitrile - in acetonitrile also gives the regioisomeric mixture of nucleosides (V) and (VI) (1).3) Acylation of ribavirin (1-?D-ribofuranosyl-1,2,4-triazole-3-carboxamide) (IX) with Ac2O and pyridine gives the triacetate (X),which is dehydrated by means of POCl3 and triethylamine in chloroform to yield 3-cyano-1-(2,3,5-tri-O-acetyl-?D-ribofuranosyl)-1,2,4-triazole (V).Treatment of nucleoside (V) with NaOMe in methanol affords the methyl carboximidate (XI),which is finally treated with NH4Cl and dry NH3 gas in methanol (3).

参考文献标题:Synthesis and antiviral activity of 1,2,4-triazole-3-thiocarboxamide and 1,2,4-triazole-3-carboxamidine ribonucleosides
文献作者:Witkowski,J.T.; Robins,R.K.; Khare,G.P.; Sidwell,R.W.
参考来源:J Med Chem 1973,16(8),935


合成路线:Viramidine can be synthesized by several related ways: 1) Reaction of triethyl orthoformate (I) with 1-cyanoformimidic acid hydrazide (II) by means of anhydrous HCl in dioxane gives 1,2,4-triazole-3-carbonitrile (III),which is condensed with tetra-O-acetyl-?D-ribofuranose (IV) by means of di-p-nitrophenyl phosphate (BNPP) at 150 oC to yield a mixture of the regioisomeric ribonucleosides (V) and (VI),easily separated by chromatography.Finally,the suitable regiosomer 3-cyano-1-(2,3,5-tri-O-acetyl-?D-ribofuranosyl)-1,2,4-triazole (V) is treated with anhydrous NH3 and NH4Cl at 85 oC in a pressure bomb (1,2).2) Alternatively,condensation of 2,3,5-tri-O-acetyl-?D-ribofuranosyl bromide (VII) with 1-(trimethylsilyl)-1,2,4-triazole-3-carbonitrile (VIII) - prepared by treatment of triazole (III) with hexamethyldisilazane in dry acetonitrile - in acetonitrile also gives the regioisomeric mixture of nucleosides (V) and (VI) (1).3) Acylation of ribavirin (1-?D-ribofuranosyl-1,2,4-triazole-3-carboxamide) (IX) with Ac2O and pyridine gives the triacetate (X),which is dehydrated by means of POCl3 and triethylamine in chloroform to yield 3-cyano-1-(2,3,5-tri-O-acetyl-?D-ribofuranosyl)-1,2,4-triazole (V).Treatment of nucleoside (V) with NaOMe in methanol affords the methyl carboximidate (XI),which is finally treated with NH4Cl and dry NH3 gas in methanol (3).

参考文献标题:Synthesis and antitumor activity of ribavirin imidates.A new facile synthesis of ribavirin amidine (1-beta-D-ribofuranosyl-1,2,4-triazole-3-carboxamidine hydrochloride)
文献作者:Kini,G.D.; Robins,R.K.; Avery,T.L.
参考来源:J Med Chem 1989,32(7),1447


合成路线:Viramidine can be synthesized by several related ways: 1) Reaction of triethyl orthoformate (I) with 1-cyanoformimidic acid hydrazide (II) by means of anhydrous HCl in dioxane gives 1,2,4-triazole-3-carbonitrile (III),which is condensed with tetra-O-acetyl-?D-ribofuranose (IV) by means of di-p-nitrophenyl phosphate (BNPP) at 150 oC to yield a mixture of the regioisomeric ribonucleosides (V) and (VI),easily separated by chromatography.Finally,the suitable regiosomer 3-cyano-1-(2,3,5-tri-O-acetyl-?D-ribofuranosyl)-1,2,4-triazole (V) is treated with anhydrous NH3 and NH4Cl at 85 oC in a pressure bomb (1,2).2) Alternatively,condensation of 2,3,5-tri-O-acetyl-?D-ribofuranosyl bromide (VII) with 1-(trimethylsilyl)-1,2,4-triazole-3-carbonitrile (VIII) - prepared by treatment of triazole (III) with hexamethyldisilazane in dry acetonitrile - in acetonitrile also gives the regioisomeric mixture of nucleosides (V) and (VI) (1).3) Acylation of ribavirin (1-?D-ribofuranosyl-1,2,4-triazole-3-carboxamide) (IX) with Ac2O and pyridine gives the triacetate (X),which is dehydrated by means of POCl3 and triethylamine in chloroform to yield 3-cyano-1-(2,3,5-tri-O-acetyl-?D-ribofuranosyl)-1,2,4-triazole (V).Treatment of nucleoside (V) with NaOMe in methanol affords the methyl carboximidate (XI),which is finally treated with NH4Cl and dry NH3 gas in methanol (3).
参考文献标题:Viramidine hydrochloride
文献作者:Cox,S.; Castar,J.
参考来源:Drugs Fut 2004,29(7),687


产品链接: CAS No. 40372-00-7››

产品链接: CAS No.119567-79-2››