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HRID 52227作成日:2026年10月24日

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

https://huagongshe.com/ja/reaction/52227

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2,3-Dichloro-5-(trifluoromethyl)pyridineHCID 112234—
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-chloro-5-trifluoromethylpyridine-2-yloxymethyl)phenyl]-3-(2-chloro-6-fluorophenyl)-1-methyl-1H-1,2,4-triazoleHCID 2146362960.7%

反応条件

温度-5 °C

反応手順

Sodium hydride (60%, 0.16 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 (1.20 g) in 1,2-dimethoxyethane (20 ml) is added dropwise thereto at -5° C. with stirring. To the reaction solution is added dropwise a solution of 2,3-dichloro-5-trifluoromethyl pyridine (0.80 g) in 1,2-dimethoxyethane (20 ml) at -5° C. for 10 minutes, which is further stirred for 15 minutes. On completion of the reaction, the reaction solution 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 1.10 g of desired compound (melting point: 47.0°-49.0° 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-e9ed4c366909416380fc24655b8be2e1
出典メモuspto-grants-1997_04