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HRID 22296作成日:2026年10月24日

Sodium hydride → 3-(2,3-Dichlorophenylthiomethyl)-5-methyl-1,2,4-oxadiazole

https://huagongshe.com/ja/reaction/22296

反応式

関与物質

役割名称HCID仕込み量
反応物Sodium hydrideHCID 24758—
反応物2,3-DichlorobenzenethiolHCID 140202—
反応物3-(Chloromethyl)-5-methyl-1,2,4-oxadiazoleHCID 302157—
溶媒TetrahydrofuranHCID 8028—
生成物3-(2,3-Dichlorophenylthiomethyl)-5-methyl-1,2,4-oxadiazoleHCID 1992865840.7%

反応手順

7.0 g (39.1 mmol) of 2,3-dichloro-thiophenol are introduced into 50 ml of absolute tetrahydrofuran, the mixture is treated with 1.2 g (0.039 mmol) of 80% sodium hydride dispersion in portions and stirred for 2 hours at reflux temperature. The mixture is subsequently treated with 4.5 g (33.9 mmol) of 3-chloromethyl-5-methyl-1,2,4-oxadiazole at room temperature and stirred until the reaction is complete (approximately 10 to 15 hours). The sodium chloride which has precipitated is subsequently separated off and the entire batch is concentrated in vacuo. The crude product which remains can be chromatographed over a silica gel column (silica gel 60-Merck, particle size: 0.040 to 0.063 mm) using toluene as the eluent. 3.8 g (36.5% of theory) of 3-(2,3-dichlorophenylthiomethyl)-5-methyl-1,2,4-oxadiazole are obtained.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05428047
出典データセットuspto-grants-1995_06
ORD IDord-bfc60d7b03054bb0bd5938345113d8c0
出典メモuspto-grants-1995_06