【药物名称】TAK-475
化学结构式(Chemical Structure):
参考文献No.32879
标题:Benzoxazepine cpds., their production and use as lipid lowering agents
作者:Yukimasa, H.; Sugiyama, Y.; Tozawa, R. (Takeda Chemical Industries, Ltd.)
来源:EP 0862562; EP 1097928; JP 1997136880; JP 2001097963; US 6110909; US 6613761; WO 9710224
合成路线图解说明:

The optically active amino benzhydrol (I) is acylated with dimethylmalonyl chloride monoethyl ester (II) to yield amide (III). Subsequent reduction of the amide-ester (III) by means of LiAlH4 furnishes amino alcohol (IV). Alternatively, the intermediate amino alcohol (IV) is prepared by reductive alkylation of (I) with 3-hydroxy-2,2-dimethylpropionaldehyde (V) in the presence of NaBH3CN. Condensation of (IV) with fumaryl chloride monoethyl ester (VI) provides amide (VII). Intramolecular cyclization of the conjugated carboxamide (VII) in the presence of K2CO3 leads to the benzoxazepine derivative (VIII). The ethyl ester group of (VIII) is then hydrolyzed under alkaline conditions to furnish acid (IX).

合成路线图解说明:

Acid (IX) is coupled to ethyl 4-piperidineacetate (X) by means of diethylphosphoryl cyanide to give amide (XI). The ethyl ester group of (XI) is then hydrolyzed to the corresponding carboxylic acid (XII) employing NaOH in ethanol. Finally, esterification of the alcohol function of (XII) with acetic anhydride in pyridine gives rise to the target acetate ester.

参考文献No.689162
标题:Synthesis of novel 4,1-benzoxazepine derivatives as squalene synthase inhibitors and their inhibition of cholesterol synthesis
作者:Miki, T.; Kori, M.; Mabuchi, H.; Tozawa, R.; Nishimoto, T.; Sugiyama, Y.; Teshima, K.; Yukimasa, H.
来源:J Med Chem 2002,45(20),4571
合成路线图解说明:

The optically active amino benzhydrol (I) is acylated with dimethylmalonyl chloride monoethyl ester (II) to yield amide (III). Subsequent reduction of the amide-ester (III) by means of LiAlH4 furnishes amino alcohol (IV). Alternatively, the intermediate amino alcohol (IV) is prepared by reductive alkylation of (I) with 3-hydroxy-2,2-dimethylpropionaldehyde (V) in the presence of NaBH3CN. Condensation of (IV) with fumaryl chloride monoethyl ester (VI) provides amide (VII). Intramolecular cyclization of the conjugated carboxamide (VII) in the presence of K2CO3 leads to the benzoxazepine derivative (VIII). The ethyl ester group of (VIII) is then hydrolyzed under alkaline conditions to furnish acid (IX).

合成路线图解说明:

Acid (IX) is coupled to ethyl 4-piperidineacetate (X) by means of diethylphosphoryl cyanide to give amide (XI). The ethyl ester group of (XI) is then hydrolyzed to the corresponding carboxylic acid (XII) employing NaOH in ethanol. Finally, esterification of the alcohol function of (XII) with acetic anhydride in pyridine gives rise to the target acetate ester.

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