Ro-136298

乙基-4-((E)-2-(5,6,7,8-四氢-5,5,8,8-四甲基-2-萘基)-1-丙烯基)苯甲酸Chemical Name: p-[(E)-2-(5,6,7,8-Tetrahydro-5,5,8,8-tetramethyl-2-naphthyl)propenyl]benzoic acid ethyl ester; (E)-4-[2-(5,6,7,8-Tetrahydro-5,5,8,8-tetramethyl-2-naphthalenyl)-1-propenyl]benzoic acid ethyl ester
CAS No. 71441-09-3
项目整合开发状态: Phase I
项目研究机构: Roche (Originator)
合成路线:The Friedel Kraft's acylation of 1,2,3,4-tetrahydro-1,1,4,4-tetramethylnaphthalene (I) with acetyl chloride by means of AlCl3 in nitrobenzene gives 2-acetyl-5,6,7,8-tetrahydro-5,5,8,8-tetramethylnaphthalene (II),which is reduced with LiAlH4 in ether yielding 5,6,7,8-tetrahydro-alpha,5,5,8,8-pentamethylnaphthalene-2-methanol (III),The reaction of (III) with PBr3 in ether - hexane affords 2-(1-bromoethyl)-5,6,7,8-tetrahydro-5,5,8,8-tetramethylnaphthalene (IV),which by reaction with triphenylphosphine in hot xylene is converted into [1-(5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthyl)ethyl]triphenylphosphonium bromide (V).Finally,this compound is submitted to a Wittig condensation with ethyl 4-formylbenzoate (VI) in hot butylene oxide.
📌 参考资料/链接:
参考文献标题:Stilbene derivs.
文献作者:Loeliger,P.(Hoffmann-La Roche,Inc.)
参考来源:US 4326055

📄 详细内容


合成路线:The Friedel Kraft's acylation of 1,2,3,4-tetrahydro-1,1,4,4-tetramethylnaphthalene (I) with acetyl chloride by means of AlCl3 in nitrobenzene gives 2-acetyl-5,6,7,8-tetrahydro-5,5,8,8-tetramethylnaphthalene (II),which is reduced with LiAlH4 in ether yielding 5,6,7,8-tetrahydro-alpha,5,5,8,8-pentamethylnaphthalene-2-methanol (III),The reaction of (III) with PBr3 in ether - hexane affords 2-(1-bromoethyl)-5,6,7,8-tetrahydro-5,5,8,8-tetramethylnaphthalene (IV),which by reaction with triphenylphosphine in hot xylene is converted into [1-(5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthyl)ethyl]triphenylphosphonium bromide (V).Finally,this compound is submitted to a Wittig condensation with ethyl 4-formylbenzoate (VI) in hot butylene oxide.

参考文献标题:RO-13-6298
文献作者:Blancafort,P.; Hopkins,S.J.; Serradell,M.N.; Castar,J.
参考来源:Drugs Fut 1983,8(5),432


合成路线:The Friedel Kraft's acylation of 1,2,3,4-tetrahydro-1,1,4,4-tetramethylnaphthalene (I) with acetyl chloride by means of AlCl3 in nitrobenzene gives 2-acetyl-5,6,7,8-tetrahydro-5,5,8,8-tetramethylnaphthalene (II),which is reduced with LiAlH4 in ether yielding 5,6,7,8-tetrahydro-alpha,5,5,8,8-pentamethylnaphthalene-2-methanol (III),The reaction of (III) with PBr3 in ether - hexane affords 2-(1-bromoethyl)-5,6,7,8-tetrahydro-5,5,8,8-tetramethylnaphthalene (IV),which by reaction with triphenylphosphine in hot xylene is converted into [1-(5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthyl)ethyl]triphenylphosphonium bromide (V).Finally,this compound is submitted to a Wittig condensation with ethyl 4-formylbenzoate (VI) in hot butylene oxide.
参考文献标题:Arotinoids,a new class of highly active retinoids
文献作者:Mayer,H.; Loeliger,P.; Bollag,W.
参考来源:Eur J Med Chem - Chim Ther 1980,15(1),9-15


产品链接: CAS No. 71441-09-3››