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HRID 1376095作成日:2026年10月25日

Water → 5-(4-chloro-phenyl)-3-methyl-1-(4-methylsulfanyl-phenyl)-1H-[1,2,4]triazole

https://huagongshe.com/reaction/1376095

反応式

関与物質

役割名称HCID仕込み量
反応物WaterHCID 962—
反応物TriethylamineHCID 8471—
反応物(4-(Methylsulfanyl)phenyl)hydrazine hydrochlorideHCID 2760977—
反応物N-(1-ethoxy-ethylidene)-4-chloro-benzamideHCID 21894670—
溶媒MethanolHCID 887—
溶媒DichloromethaneHCID 6344—
生成物5-(4-chloro-phenyl)-3-methyl-1-(4-methylsulfanyl-phenyl)-1H-[1,2,4]triazoleHCID 2189468459,085.102%

反応手順

N-(1-ethoxy-ethylidene)-4-chloro benzamide 472 mg (2.09 mmol) was dissolved in a mixed solvent of dichloromethane 20 ml and methanol 10 ml, and (4-methylsulfanyl-phenyl)-hydrazine hydrochloride 439 mg (2.23 mmol) was added to the solution. Then, triethylamine 0.35 ml (2.51 mmol) was slowly added dropwise at room temperature for 10 minutes and stirred for 8 hours. After completing the reaction, water 20 ml was added to the reacting solution and extracted two times with dichloromethane and then, the collected organic layer was washed with saturated brine. The organic layer was dried with anhydrous magnesium sulfate, filtered and concentrated under reduced pressure, and the resulting product was purified through a flash column chromatography (ethyl acetate:normal hexane=1:1). As a result, 5-(4-chloro-phenyl)-3-methyl-1-(4-methylsulfanyl-phenyl)-1H-[1,2,4]triazole (390 g, yield: 59%) was obtained as a liquid phase.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07169929B2
出典データセットuspto-grants-2007_01
ORD IDord-327b2df9afa9428ab67b0dcd754169c0
出典メモuspto-grants-2007_01