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HRID 588814作成日:2026年10月25日

Sodium Carbonate → 2',5',6-Trichloro-4-methoxy-[1,1'-biphenyl]-3-amine

https://huagongshe.com/reaction/588814

反応式

関与物質

役割名称HCID仕込み量
反応物Sodium CarbonateHCID 10340—
反応物2,5-Dichlorobenzeneboronic acidHCID 2773371—
反応物4-Chloro-5-iodo-2-methoxyanilineHCID 91758377—
触媒HCID 178418397HCID 178418397—
溶媒WaterHCID 962—
溶媒1,4-DioxaneHCID 31275—
生成物2',5',6-Trichloro-4-methoxy-[1,1'-biphenyl]-3-amineHCID 9045588775.8%

反応条件

温度80 °C

反応手順

A mixture of 4-chloro-5-iodo-2-methoxybenzenamine (4.1 g, 14.5 mmol), 2,5-dichlorophenylboronic acid (3.3 g, 17.4 mmol), Pd(PPh3)4 (500 mg, 1.45 mmol) and Na2CO3 (4.7 g, 43.5 mmol) in 1,4-dioxane (150 mL) and water (15 mL) was stirred at 80° C. under argon for 16 h. The mixture was allowed to cool to room temperature, and then partitioned between ethyl acetate and water. The organic layer was washed with brine, dried over Na2SO4 and concentrated in vacuo. The residue was purified by flash column chromatography on silica gel (petroleum ether/ethyl acetate=20:1) to afford the desired product (3.3 g, 75.8% yield) as an off-white solid.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09227978B2
出典データセットuspto-grants-2016_01
ORD IDord-17ba0b5f9ac646d1aa09009a88c295b6
出典メモuspto-grants-2016_01