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HRID 52226作成日:2026年10月23日

Water → 5-[3-chloro-4-(3,5-dichloropyridine-2-yloxymethyl)phenyl]-3-(2-chloro-6-fluorophenyl)-1-methyl-1H-1,2,4-triazole

https://huagongshe.com/ja/reaction/52226

反応式

関与物質

役割名称HCID仕込み量
反応物WaterHCID 962—
反応物Sodium hydrideHCID 24758—
反応物Pyridine, 2,3,5-trichloro-HCID 27666—
反応物3-(2-chloro-6-fluorophenyl)-5-(3-chloro 4-hydroxymethylphenyl)-1-methyl-1H-1,2,4-triazoleHCID 21463672—
溶媒1,2-DimethoxyethaneHCID 8071—
生成物5-[3-chloro-4-(3,5-dichloropyridine-2-yloxymethyl)phenyl]-3-(2-chloro-6-fluorophenyl)-1-methyl-1H-1,2,4-triazoleHCID 2146364928.3%

反応条件

温度-5 °C

反応手順

Sodium hydride (60%, 0.12 g) is added to 1,2-dimethoxyethane (50 ml) and a solution of 3-(2-chloro-6-fluorophenyl)-5-(3-chloro-4-hydroxymethylphenyl) 1-methyl-1H-1,2,4-triazole (1.00 g) in 1,2-dimethoxyethane (20 ml) is added dropwise thereto at -5° C. and stirred for 20 minutes. The reaction solution is added dropwise with a solution of 2,3,5-trichloropyridine (0.60 g) in 1,2-dimethoxyethane (20 ml) at -5° C. for 10 minutes with stirring. The reaction mixture is warmed to room temperature, poured into water and extracted with ethyl acetate. The organic layer is washed with water, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The concentrate is purified by silica gel column chromatography to give 0.40 g of desired compound (melting point: 153.0°-155.0° C.).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05616594
出典データセットuspto-grants-1997_04
ORD IDord-82f3a818f4704e989865071da7e7785b
出典メモuspto-grants-1997_04