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HRID 218537作成日:2026年10月25日

Water → 1-(5-Chloro-2-methyl-4-nitrophenyl)-3-methylpyridin-2(1H)-one

https://huagongshe.com/reaction/218537

反応式

関与物質

役割名称HCID仕込み量
反応物WaterHCID 962—
反応物4-Chloro-2-fluoro-5-nitrotolueneHCID 87593—
反応物Potassium tert-butoxideHCID 23665647—
反応物HCID 178426317HCID 178426317—
溶媒DimethylformamideHCID 6228—
生成物1-(5-Chloro-2-methyl-4-nitrophenyl)-3-methylpyridin-2(1H)-oneHCID 59586695—

反応手順

1.50 g (13.8 mmol) of 2-hydroxy-3-methylpyridine in 70 ml of DMF are admixed at 0° C. with 2.31 g (20.6 mmol) of potassium tert-butoxide, and the mixture is stirred at room temperature for 30 min. 2.87 g (15.1 mmol) of 2-chloro-4-fluoro-5-methylnitrobenzene are added while continuing to stir at RT. After 17 h, the mixture is admixed with 1000 ml of water and then extracted three times with ethyl acetate. The combined organic phases are dried over sodium sulfate and, after filtration, the solvents are removed under reduced pressure. The residue is purified by chromatography on silica gel (2:1 cyclohexane/ethyl acetate). This affords 2.15 g (56% of theory) of the desired compound.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08198267B2
出典データセットuspto-grants-2012_06
ORD IDord-babfbf2138ce4c39855e0fa8fe8bc918
出典メモuspto-grants-2012_06