反应详情

温度

30 °C

2.36 g of 2,3,4-trimethoxy-6-methylbromobenzene and 0.32 g of agnesium turnings were initially charged in 5 ml of anhydrous tetrahydrofuran, 0.57 ml of 1,2-dibromoethane was added and the reaction mixture was heated at reflux temperature for about 40 min. After cooling to 30° C., 1.40 g of 5-bromo-2-methoxy-6-methylbenzaldehyde were added dropwise, and the solution was stirred for about two hours. Water/2N hydrochloric acid (1/1) was added, the aqueous phase was extracted with ethyl acetate, the organic phases were washed with water and dried and the solvent was distilled off, and the residue was then purified by column chromatography (mobile phase petroleum ether/ethyl acetate 85/5). 1.5 g of the title compound were isolated as a violet viscous oil.

1. temperaturethe reaction mixture was heated
2. temperatureat reflux temperature for about 40 min
3. extractionthe aqueous phase was extracted with ethyl acetate
4. washthe organic phases were washed with water
5. customdried
6. distillationthe solvent was distilled off
7. customthe residue was then purified by column chromatography (mobile phase petroleum ether/ethyl acetate 85/5)