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HRID 85231作成日:2026年10月24日

Sodium Chloride → 1-(2,6-Dimethyl-4-nitrophenyl)-3-methoxypyridin-2(1H)-one

https://huagongshe.com/ja/reaction/85231

反応式

関与物質

役割名称HCID仕込み量
反応物Sodium ChlorideHCID 5234—
反応物3-Methoxy-2-pyridoneHCID 88731—
反応物1-Fluoro-2,5-dimethyl-4-nitrobenzeneHCID 23234438—
反応物Potassium tert-butoxideHCID 23665647—
溶媒WaterHCID 962—
溶媒DimethylformamideHCID 6228—
生成物1-(2,6-Dimethyl-4-nitrophenyl)-3-methoxypyridin-2(1H)-oneHCID 59410213—

反応手順

At 0° C., 452 mg (4.03 mmol) of potassium tert-butoxide are added to 336 mg (2.69 mmol) of 3-methoxypyridinone in 10 ml of DMF, and the mixture is stirred at room temperature for 30 min. 500 mg (2.96 mmol) of 1-fluoro-2,5-dimethyl-4-nitrobenzene are added, and the mixture is stirred at 80° C. After 22 h, the mixture is heated at 120° C. and stirred for a further 20 h. The mixture is then cooled and added to 100 ml of water and 15 ml of saturated aqueous sodium chloride solution. The mixture is extracted three times with in each case 300 ml of ethyl acetate, and the combined organic phases are dried over sodium sulphate. After filtration, the solvents are removed under reduced pressure and the residue is purified by chromatography on silica gel (cyclohexane/ethyl acetate 1:1). This gives 383 mg (52% of theory) of the desired compound.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08846934B2
出典データセットuspto-grants-2014_09
ORD IDord-00c5fd4c2a594e26b59589a8b3dbe3c7
出典メモuspto-grants-2014_09