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HRID 38203作成日:2026年10月26日

2-Bromo-1-fluoro-4-nitrobenzene → 2-Bromo-1-methylsulfanyl-4-nitrobenzene

https://huagongshe.com/reaction/38203

反応式

関与物質

役割名称HCID仕込み量
反応物2-Bromo-1-fluoro-4-nitrobenzeneHCID 69699—
反応物Sodium methanethiolateHCID 4378561—
溶媒DimethylformamideHCID 6228—
生成物2-Bromo-1-methylsulfanyl-4-nitrobenzeneHCID 59550842—

反応条件

温度60 °C

反応手順

A solution of 25.7 g (120 mmol) 2-bromo-1-fluoro-4-nitrobenzene in 154 ml DMF is treated with 10.6 g (150 mmol) sodium thiomethylate and stirred for 5 hours at 60° C. The mixture is stirred at room temperature for 18 hours, again treated with 1.0 g sodium thiomethylate and stirred for a further 6 hours at 60° C. After cooling, the mixture is poured into ice-water and extracted with ethyl acetate (3×). The combined organic phases are washed with water, dried (Na2SO4), filtered and concentrated. The residue obtained is chromatographically purified (hexane/ethyl acetate 2:1). 20.4 g (82 mmol, corresponding to 70% of theor.) of the product is obtained.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08524724B2
出典データセットuspto-grants-2013_09
ORD IDord-ba4198057e124a7d9fb4280a99667f3b
出典メモuspto-grants-2013_09