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HRID 13522作成日:2026年10月25日

Potassium Carbonate → 4-(4-Amino-3-nitro-phenoxy)-pyridine-2-carboxylic acid dimethylamide

https://huagongshe.com/reaction/13522

反応式

関与物質

役割名称HCID仕込み量
反応物Potassium CarbonateHCID 11430—
反応物Potassium bis(trimethylsilyl)amideHCID 3251421—
反応物4-Amino-3-NitrophenolHCID 3758882—
反応物4-chloro-N,N-dimethylpyridine-2-carboxamideHCID 4962252—
溶媒DimethylformamideHCID 6228—
生成物4-(4-Amino-3-nitro-phenoxy)-pyridine-2-carboxylic acid dimethylamideHCID 21037294—

反応条件

温度90 °C

反応手順

A mixture containing 4-amino-3-nitrophenol (1 eq) and potassium bis(trimethylsilyl)amide (2 eq) was stirred in dimethylformamide for 2 hours at room temperature. To this mixture was added 4-Chloro-pyridine-2-carboxylic acid dimethylamide (1 eq) and potassium carbonate (1.2 eq) and then it was stirred at 90° C. for 3 days. The reaction mixture was then concentrated before partitioning between ethyl acetate and water. The organic layer was separated, washed with brine, dried, filtered and concentrated in vacuum to give brown solid. Purification by flash chromatography with ethyl acetate and hexane (1:1) gave the desired product as a yellow syrup. HPLC, 1.69 min; MS: MH+=303.1.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07728010B2
出典データセットuspto-grants-2010_06
ORD IDord-2ce32362d15346048dc575b0b0923ee7
出典メモuspto-grants-2010_06