KCO-616, WAY-151616

Chemical Name: 3-(2,4-Dichloro-6-methylbenzylamino)-4-(1,1-dimethylpropylamino)-3-cyclobutene-1,2-dione
CAS No. 202520-55-6
项目整合开发状态: Preclinical
项目研究机构: Wyeth Pharmaceuticals (Originator)
合成路线:A general synthetic route to a series of novel N-aryl and N-benzyl diaminocyclobutenedione derivatives and pertinent SAR data have been reported elsewhere.KCO-616 can be conveniently synthesized in two steps as shown in Scheme 26121401a.An ethanolic solution of 3,4-diethoxy-3-cyclobutene-1,2-dione (I) is allowed to react with tert-amylamine (II) at room temperature for a period of 24 h to give intermediate 3-(1,1-dimethylpropylamino)-4-ethoxy-3-cyclobutene-1,2-dione (III) in 90% isolated,purified yield.The condensation of this compound with 2,4-dichloro-6-methylbenzylamine (IV,recrystallized from boiling diethyl ether) in ethanol at room temperature for 24 h affords analytically pure 3-(2,4-dichloro-6-methylbenzylamino)-4-(1,1-dimethylpropylamino)-3-cyclobutene-1,2-dione (KCO-616) in 92% yield.

合成路线:Benzylic bromination of 3-chloro-4-methylbenzonitrile (I) by means of N-bromosuccinimide and azobis(isobutyronitrile) provided bromide (II).Subsequent displacement of the bromine atom of (III) by potassium phthalimide (III) afforded the N-substituted phthalimide (IV),which was then deprotected with ethanolic hydrazine to furnish the primary amine (V).

合成路线:Treatment of 3,4-dibutoxy-3-cyclobutene-1,2-dione (VI) with tert-butylamine (VII) yielded the amino cyclobutenedione (VIII).Subsequent condensation of (VIII) with 3-chloro-4-(aminomethyl)benzonitrile (V) in THF provided the target diamino derivative.

合成路线:Benzylic bromination of 3-chloro-4-methylbenzonitrile (I) by means of N-bromosuccinimide and azobis(isobutyronitrile) provided bromide (II).Subsequent displacement of the bromine atom of (II) by potassium phthalimide (III) afforded the N-substituted phthalimide (IV),which was then deprotected with ethanolic hydrazine to furnish the primary amine (V).

合成路线:Treatment of 3,4-dibutoxy-3-cyclobutene-1,2-dione (VI) with 1,1-dimethylpropylamine (VII) yielded the amino cyclobutenedione (VIII).Subsequent condensation of (VIII) with 3-chloro-4-(aminomethyl)benzonitrile (V) in THF provided the target diamino derivative.
📌 参考资料/链接:
参考文献标题:Substd.N-arylmethylamino derivs.of cyclobutene-3,4-diones
文献作者:Antane,M.M.; Herbst,D.R.; McFarlane,G.R.; Gundersen,E.G.; Hirth,B.H.; Quagliato,D.A.; Graceffa,R.F.; Butera,J.A.; Gilbert,A.M.(American Home Products Corp.)
参考来源:US 5763474; US 5780505; WO 9802413

📄 详细内容


合成路线:A general synthetic route to a series of novel N-aryl and N-benzyl diaminocyclobutenedione derivatives and pertinent SAR data have been reported elsewhere.KCO-616 can be conveniently synthesized in two steps as shown in Scheme 26121401a.An ethanolic solution of 3,4-diethoxy-3-cyclobutene-1,2-dione (I) is allowed to react with tert-amylamine (II) at room temperature for a period of 24 h to give intermediate 3-(1,1-dimethylpropylamino)-4-ethoxy-3-cyclobutene-1,2-dione (III) in 90% isolated,purified yield.The condensation of this compound with 2,4-dichloro-6-methylbenzylamine (IV,recrystallized from boiling diethyl ether) in ethanol at room temperature for 24 h affords analytically pure 3-(2,4-dichloro-6-methylbenzylamino)-4-(1,1-dimethylpropylamino)-3-cyclobutene-1,2-dione (KCO-616) in 92% yield.

参考文献标题:Substituted N-aryl-1,2-diaminocyclobutene-3,4-diones.I.N-Cyanoguanidine bioisosteres possessing in vivo bladder selectivity
文献作者:Butera,J.A.; et al.
参考来源:214th ACS Natl Meet (Sept.7-11,Las Vegas) 1997,Abst MEDI 044


合成路线:A general synthetic route to a series of novel N-aryl and N-benzyl diaminocyclobutenedione derivatives and pertinent SAR data have been reported elsewhere.KCO-616 can be conveniently synthesized in two steps as shown in Scheme 26121401a.An ethanolic solution of 3,4-diethoxy-3-cyclobutene-1,2-dione (I) is allowed to react with tert-amylamine (II) at room temperature for a period of 24 h to give intermediate 3-(1,1-dimethylpropylamino)-4-ethoxy-3-cyclobutene-1,2-dione (III) in 90% isolated,purified yield.The condensation of this compound with 2,4-dichloro-6-methylbenzylamine (IV,recrystallized from boiling diethyl ether) in ethanol at room temperature for 24 h affords analytically pure 3-(2,4-dichloro-6-methylbenzylamino)-4-(1,1-dimethylpropylamino)-3-cyclobutene-1,2-dione (KCO-616) in 92% yield.

参考文献标题:Benzylamino analogs of 1,2-diaminocyclobutene-3,4-dione as novel KATP-channel openers targeted for treatment of urge urinary incontinence
文献作者:McFarlane,G.R.; Gundersen,E.G.; Elokdah,H.; et al.
参考来源:218th ACS Natl Meet (Aug 22 1999,New Orleans) 1999,Abst MEDI 35


合成路线:A general synthetic route to a series of novel N-aryl and N-benzyl diaminocyclobutenedione derivatives and pertinent SAR data have been reported elsewhere.KCO-616 can be conveniently synthesized in two steps as shown in Scheme 26121401a.An ethanolic solution of 3,4-diethoxy-3-cyclobutene-1,2-dione (I) is allowed to react with tert-amylamine (II) at room temperature for a period of 24 h to give intermediate 3-(1,1-dimethylpropylamino)-4-ethoxy-3-cyclobutene-1,2-dione (III) in 90% isolated,purified yield.The condensation of this compound with 2,4-dichloro-6-methylbenzylamine (IV,recrystallized from boiling diethyl ether) in ethanol at room temperature for 24 h affords analytically pure 3-(2,4-dichloro-6-methylbenzylamino)-4-(1,1-dimethylpropylamino)-3-cyclobutene-1,2-dione (KCO-616) in 92% yield.

参考文献标题:KCO-616
文献作者:Butera,J.A.; Argentieri,T.M.
参考来源:Drugs Fut 2000,25(3),239


合成路线:A general synthetic route to a series of novel N-aryl and N-benzyl diaminocyclobutenedione derivatives and pertinent SAR data have been reported elsewhere.KCO-616 can be conveniently synthesized in two steps as shown in Scheme 26121401a.An ethanolic solution of 3,4-diethoxy-3-cyclobutene-1,2-dione (I) is allowed to react with tert-amylamine (II) at room temperature for a period of 24 h to give intermediate 3-(1,1-dimethylpropylamino)-4-ethoxy-3-cyclobutene-1,2-dione (III) in 90% isolated,purified yield.The condensation of this compound with 2,4-dichloro-6-methylbenzylamine (IV,recrystallized from boiling diethyl ether) in ethanol at room temperature for 24 h affords analytically pure 3-(2,4-dichloro-6-methylbenzylamino)-4-(1,1-dimethylpropylamino)-3-cyclobutene-1,2-dione (KCO-616) in 92% yield.

参考文献标题:Desing and SAR of novel potassium channel openers targeted for urge urinary incontinence.2.Selective and potent benzylamino cyclobutenediones
文献作者:Gilbert,A.M.; Antane,M.M.; Argentieri,T.M.; Butera,J.A.; Francisco,G.D.; Freeden,C.; Gundersen,E.G.; Graceffa,R.F.; Herbst,D.; Hirth,B.H.; Lennox,J.R.; McFarlane,G.; Norton,N.W.; Quagliato,D.; Sheldon,J.H.; Warga,D.; Wojdan,A.; Woods,M.
参考来源:J Med Chem 2000,43(6),1203


合成路线:A general synthetic route to a series of novel N-aryl and N-benzyl diaminocyclobutenedione derivatives and pertinent SAR data have been reported elsewhere.KCO-616 can be conveniently synthesized in two steps as shown in Scheme 26121401a.An ethanolic solution of 3,4-diethoxy-3-cyclobutene-1,2-dione (I) is allowed to react with tert-amylamine (II) at room temperature for a period of 24 h to give intermediate 3-(1,1-dimethylpropylamino)-4-ethoxy-3-cyclobutene-1,2-dione (III) in 90% isolated,purified yield.The condensation of this compound with 2,4-dichloro-6-methylbenzylamine (IV,recrystallized from boiling diethyl ether) in ethanol at room temperature for 24 h affords analytically pure 3-(2,4-dichloro-6-methylbenzylamino)-4-(1,1-dimethylpropylamino)-3-cyclobutene-1,2-dione (KCO-616) in 92% yield.

合成路线:The condensation of 4-amino-3-ethylbenzonitrile (I) with 3,4-diethoxy-3-cyclobutene-1,2-dione (II) in refluxng acetonitrile gives 4-(2-ethoxy-3,4-dioxo-1-cyclobutenylamino)-3-ethylbenzonitrile (III),which is finally condensed with (R)-1,2,2-trimethylpropylamine (IV) in ethanol.
参考文献标题:Design and SAR of novel potassium channel openers targeted for urge urinary incontinence.I.N-Cyanoguanidine bioisosteres possessing in vivo bladder selectivity
文献作者:Butera,J.A.; Antane,M.M.; Antane,S.A.; Argentieri,T.M.; Freeden,C.; Graceffa,R.F.; Hirth,B.H.; Jenkins,D.; Lennox,J.R.; Matelan,E.; Norton,N.W.; Quagliato,D.; Sheldon,J.H.; Spinelli,W.; Warga,D.; Wojdan,A.; Woods,M.
参考来源:J Med Chem 2000,43(6),1187-1202


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