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HRID 6931作成日:2026年10月24日

Chloroform → 2-{3-[N-(2-Methoxyethyl)-N-methylamino]-5-(6-phenylpyridin-3-yl)-4H-1,2,4-triazol-4-yl}benzonitrile

https://huagongshe.com/ja/reaction/6931

反応式

関与物質

役割名称HCID仕込み量
反応物ChloroformHCID 6212—
反応物N-methyl-2-pyrrolidoneHCID 13387—
反応物Calcium HydroxideHCID 6093208—
反応物[4-(2-Bromophenyl)-5-(6-phenylpyridin-3-yl)-4H-1,2,4-triazol-3-yl]-N-(2-methoxyethyl)-N-methylamineHCID 22019250—
触媒Zinc cyanide (Zn(CN)2)HCID 11186—
生成物2-{3-[N-(2-Methoxyethyl)-N-methylamino]-5-(6-phenylpyridin-3-yl)-4H-1,2,4-triazol-4-yl}benzonitrileHCID 1029503463%

反応条件

温度180 °C

反応手順

[4-(2-Bromophenyl)-5-(6-phenylpyridin-3-yl)-4H-1,2,4-triazol-3-yl]-N-(2-methoxyethyl)-N-methylamine (436 mg) prepared in the Example 7 was dissolved in N-methyl-2-pyrrolidone (5 ml), followed by addition of zinc cyanide (121 mg), calcium hydroxide (76 mg) and tetrakistriphenylphosphine palladium (326 mg), and stirred at 180° C. for 3 hours. After the reaction solution was cooled to ambient temperature, chloroform was added to the solution, from which insoluble materials were filtered off. The filtrate was washed with saturated aqueous sodium hydrogen carbonate solution, and the organic layer was dried over anhydrous magnesium sulfate. After the solvent was evaporated under reduced pressure, the resulting solid was recrystallized from ethyl acetate, to afford the entitled compound as white crystal (242 mg, 63%). The physico-chemical values are as follows.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07084164B2
出典データセットuspto-grants-2006_08
ORD IDord-b5c95ac0d15845fe92f518839e0e9db3
出典メモuspto-grants-2006_08