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HRID 37497作成日:2026年10月26日

Dimethylformamide → 2-Chloro-3,4-diethoxycarbonyl-5-nitro-6-phenylpyridine

https://huagongshe.com/reaction/37497

反応式

関与物質

役割名称HCID仕込み量
反応物DimethylformamideHCID 6228—
反応物Phosphorus oxychlorideHCID 24813—
反応物Diethyl 2-hydroxy-5-nitro-6-phenylpyridine-3,4-dicarboxylateHCID 19935597—
生成物2-Chloro-3,4-diethoxycarbonyl-5-nitro-6-phenylpyridineHCID 19935587—

反応条件

温度100 °C

反応手順

In 6.5 ml of phosphorus oxychloride was dissolved 2.5 g of 3,4-diethoxycarbonyl-5-nitro-6-phenyl-2pyridone, followed by addition of 1 ml of DMF. The mixture was heated at 100° C. for 30 minutes. After the reaction mixture was concentrated under reduced pressure, an aqueous solution of sodium hydrogencarbonate was added to the residue for neutralization, followed by extraction with ethyl acetate. The organic layer was washed with water and a saturated aqueous solution of sodium chloride and dried over magnesium sulfate. After the solvent was distilled off, the residue was subjected to silica gel column chromatography (eluent:ethyl acetate/hexane 1:2), to give 1.9 g of the title compound as yellow needles.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05420275
出典データセットuspto-grants-1995_05
ORD IDord-e1042bcf07c04ef68cc62404a8ba4b14
出典メモuspto-grants-1995_05