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HRID 245290作成日:2026年10月25日

Tetramethyltin → 4-Acetylamino-6-(4-chloro-2-fluoro-3-methoxyphenyl)-3-methylpyridine-2-carboxylic acid methyl ester

https://huagongshe.com/reaction/245290

反応式

関与物質

役割名称HCID仕込み量
反応物TetramethyltinHCID 11661—
反応物Methyl 4-(acetylamino)-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)pyridine-2-carboxylateHCID 67210962—
触媒HCID 178418476HCID 178418476—
溶媒AcetonitrileHCID 6342—
生成物4-Acetylamino-6-(4-chloro-2-fluoro-3-methoxyphenyl)-3-methylpyridine-2-carboxylic acid methyl esterHCID 5943212788.6%

反応条件

温度110 °C

反応手順

4-Acetylamino-3-chloro-6-(4-chloro-2-fluoro-3-methoxyphenyl)-pyridine-2-carboxylic acid methyl ester (500 mg, 1.29 mmol), tetramethyltin (924 mg, 5.17 mmol), bis(triphenylphosphine)palladium(II) dichloride (91 mg, 0.129 mmol), and tetrabutylammonium triphenyldifluorosilicate (1.395 g, 2.58 mmol) were combined in 2 mL of acetonitrile and heated in a CEM microwave reactor at 110° C. for 15 min. The resulting reaction mixture was filtered and concentrated. This intermediate product was purified by flash chromatography on silica gel (ethyl acetate/hexane gradient) to yield the title compound (419 mg, 88% yield). mp 182-184° C.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08658791B2
出典データセットuspto-grants-2014_02
ORD IDord-6dbffbc9a2b046a88853e735a257edb0
出典メモuspto-grants-2014_02