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HRID 1387529作成日:2026年10月27日

Mesitylene → 3-[Acetyl-(3,5-dichlorophenyl)-amino]-4-methoxybenzoic acid methyl ester

https://huagongshe.com/reaction/1387529

反応式

関与物質

役割名称HCID仕込み量
反応物MesityleneHCID 7947—
反応物Ethyl AcetateHCID 8857—
反応物Benzene, 1-bromo-3,5-dichloro-HCID 29766—
反応物Sodium BicarbonateHCID 516892—
反応物Methyl 2-acetamido-4-methoxybenzoateHCID 54415798—
触媒Copper iodideHCID 83717—
生成物3-[Acetyl-(3,5-dichlorophenyl)-amino]-4-methoxybenzoic acid methyl esterHCID 54300158—

反応手順

A mixture of 2-acetylamino-4-methoxybenzoic acid methyl ester (9.58 g, 42.92 mmol), 1-bromo-3,5-dichlorobenzene (28.80 g, 127.48 mmol), copper iodide (2.32 g, 12.18 mmol), and sodium bicarbonate (8.72 g, 103.80 mmol) in of mesitylene (60 mL) was heated to reflux. After 7 days, the mixture was allowed to cool and was diluted with ethyl acetate (300 mL). The resulting solid was removed by filtration and washed with ethyl acetate. The filtrate was concentrated in vacuo and the residue was chromatographed on silica gel eluting with hexane/ethyl acetate (9:1→1:1) to afford the product (11.6 g); m.p. 100-101° C. after trituration in hexane.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US06268387B1
出典データセットuspto-grants-2001_07
ORD IDord-756f52fcbc6e470d8dd0e668fcf7c965
出典メモuspto-grants-2001_07