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HRID 368292作成日:2026年10月27日

Water → 3-Ethyl-5-(5-chloro-6-methylthio-3-pyridyl)-isoxazole

https://huagongshe.com/reaction/368292

反応式

関与物質

役割名称HCID仕込み量
反応物WaterHCID 962—
反応物1-NitropropaneHCID 7903—
反応物1,4-DiisocyanatobenzeneHCID 61009—
反応物3-Chloro-5-ethynyl-2-methylthiopyridineHCID 23288266—
触媒TriethylamineHCID 8471—
溶媒BenzeneHCID 241—
生成物3-Ethyl-5-(5-chloro-6-methylthio-3-pyridyl)-isoxazoleHCID 23288273479.8%

反応手順

A mixture of 3-chloro-5-ethynyl-2-methylthiopyridine (0.5 g, 2.72 mmol), 1-nitropropane (0.24 g, 0.27 mmol), 1,4-phenylenediisocyanate (1.3 g, 7.93 mmol) and triethylamine (5 drops) in benzene (20 mL) was heated under reflux with stirring for 8 hours, and allowed to stir at room temperature overnight. Water (1 mL) was added and the mixture stirred at room temperature for 2 hours. It was filtered through Celite, dried over anhydrous sodium sulphate and evaporated under reduced pressure. Recrystallisation of the residue from hexane gave the desired product (0.33 g, 48%) as a cream solid, melting point. 78-80° C.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US06133294
出典データセットuspto-grants-2000_10
ORD IDord-fde49c4efa35456d916553572faf7e32
出典メモuspto-grants-2000_10