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HRID 54025作成日:2026年10月25日

Hexane → 2-Bromo-1,3-dimethoxybenzene

https://huagongshe.com/reaction/54025

反応式

関与物質

役割名称HCID仕込み量
反応物HexaneHCID 8058—
反応物1,3-DimethoxybenzeneHCID 9025—
反応物Carbon tetrabromideHCID 11205—
反応物ButyllithiumHCID 178418339—
溶媒WaterHCID 962—
溶媒Diethyl EtherHCID 3283—
溶媒Ethyl AcetateHCID 8857—
生成物2-Bromo-1,3-dimethoxybenzeneHCID 61229657.3%

反応条件

温度0 °C

反応手順

In a solution of 1,3-dimethoxybenzene (3.0 g, 21.7 mmol) dissolved in diethyl ether (90 ml), a 1.65M solution of n-butyl lithium in n-hexane (19.8 ml, 32.7 mmol of n-butyl lithium) was added at room temperature, and a reaction mixture was heated to reflux for 4 hours. After cooling the reaction mixture to 0° C., a solution of carbon tetrabromide (15.8 g, 47.7 mmol) in diethyl ether (60 ml) was added to the mixture, and stirred at room temperature for 20 hours. A small amount of water was added to the reaction mixture, and then the reaction mixture was diluted with ethyl acetate (90 ml). The organic layer was washed with water and dried over anhydrous magnesium sulfate. Thereafter, the solvent was evaporated off, and the residue was purified by column chromatography to obtain 1-bromo-2,6-dimethoxybenzene (2.70 g).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05621129
出典データセットuspto-grants-1997_04
ORD IDord-fc9b38681b0e43a0aaebc84a04652613
出典メモuspto-grants-1997_04