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Tigilcycline, Tigecycline, WAY-GAR-936, GAR-936, TBG-MINO, Tygacil

替加环素Chemical Name: (4S,4aS,5aR,12aS)-9-(N-tert-Butyl-glycylamino)-4,7-bis(dimethylamino)-3,10,12,12a-tetrahydroxy-1,11-dioxo-1,4,4a,5,5a,6,11,12-octahydronaphthacene-2-carboxamide; 9-(N-tert-Butylglycylamido)-6-demethyl-6-deoxy-7-(dimethylamino)tetracycline
CAS No. 220620-09-7
项目整合开发状态: Phase III
项目研究机构: Wyeth Pharmaceuticals (Originator)
合成路线:Nitration of minocycline (I) with KNO3 and H2SO4 gives the 9-nitro derivative (II),which is reduced with H2 over Pd/C in 2-methoxyethanol/2N H2SO4 to provide 9-aminominocycline (III).Acylation of compound (III) with 2-bromoacetyl bromide (IV) in N,N-dimethylpropyleneurea (DMPU) affords 9-(2-bromoacetamido)minocycline (V).Finally,this compound is treated with tert-butylamine (VI) to yield,after purification,GAR-936.
📌 参考资料/链接:
参考文献标题:Method of producing 7-(substd.)-9-[(substd.glycyl)amidol]-6-demethyl-6-deoxytetracyclines
文献作者:Sum,P.-E.; Lee,V.J.(American Cyanamid Co.)
参考来源:EP 0582790; US 5284963

📄 详细内容


合成路线:By acylation of 9-amino-6-demethyl-6-deoxytetracycline (I) with sarcosyl chloride (II) by means of Na2CO3 in acetonitrile with or without dimethylpropylenurea.

合成路线:This compound can be obtained by two related ways:1) The nitration of minocycline (I) by means of NaNO3 and H2SO4 gives the 9-nitro derivative (II),which is hydrogenated with H2 over Pd/C in 2-methoxyethanol to yield the 9-amino derivative (III).Finally,this compound is acylated with sarcosyl chloride (IV) by means of Na2CO3 in acetonitrile/dimethylpropylenurea.2) The acylation of the 9-amino derivative (III) with N-(succinimidyloxycarbonyl)carbamic acid tert-butyl ester (V) by means of sodium acetate in THF gives the 9-(tert-butoxycarbonyl)glycylamino substituted compound (VI),which is deprotected with trifluoroacetic acid to afford the 9-glycylamino compound (VII).Finally,this compound is methylated with formaldehyde and simultaneous hydrogenation with H2 over Pd/C in 2-methoxyethanol.

合成路线:Nitration of minocycline (I) with KNO3 and H2SO4 gives the 9-nitro derivative (II),which is reduced with H2 over Pd/C in 2-methoxyethanol/2N H2SO4 to provide 9-aminominocycline (III).Acylation of compound (III) with 2-bromoacetyl bromide (IV) in N,N-dimethylpropyleneurea (DMPU) affords 9-(2-bromoacetamido)minocycline (V).Finally,this compound is treated with tert-butylamine (VI) to yield,after purification,GAR-936.

参考文献标题:Glycylcyclines.1.A new generation of potent antibacterial agents through modification of 9-aminotetracyclines
文献作者:Sum,P.-E.; Lee,V.J.; Testa,R.T.; Hlavka,J.J.; Ellestad,G.A.; Bloom,J.D.; Gluzman,Y.; Tally,F.P.
参考来源:J Med Chem 1994,37(1),184-8


合成路线:Nitration of minocycline (I) with KNO3 and H2SO4 gives the 9-nitro derivative (II),which is reduced with H2 over Pd/C in 2-methoxyethanol/2N H2SO4 to provide 9-aminominocycline (III).Acylation of compound (III) with 2-bromoacetyl bromide (IV) in N,N-dimethylpropyleneurea (DMPU) affords 9-(2-bromoacetamido)minocycline (V).Finally,this compound is treated with tert-butylamine (VI) to yield,after purification,GAR-936.

参考文献标题:Synthesis and structure-activity relationship of novel glycylcline derivatives leading to the discovery of GAR-936
文献作者:Sum,P.-E.; Petersen,P.
参考来源:Bioorg Med Chem Lett 1999,9(10),1459


合成路线:Nitration of minocycline (I) with KNO3 and H2SO4 gives the 9-nitro derivative (II),which is reduced with H2 over Pd/C in 2-methoxyethanol/2N H2SO4 to provide 9-aminominocycline (III).Acylation of compound (III) with 2-bromoacetyl bromide (IV) in N,N-dimethylpropyleneurea (DMPU) affords 9-(2-bromoacetamido)minocycline (V).Finally,this compound is treated with tert-butylamine (VI) to yield,after purification,GAR-936.
参考文献标题:GAR-936
文献作者:Hunter,P.A.; Castar,J.
参考来源:Drugs Fut 2001,26(9),851


产品链接: CAS No. 220620-09-7››