反应详情

A solution of crude 5-bromo-2-(7-bromoheptyloxy)-1,3-dimethylbenzene (7.81 g) in methanol (78 ml) was treated with 28% sodium methoxide in methanol (78 ml), and the solution was refluxed for 8 hours. After cooling, the reaction mixture was evaporated under reduced pressure, and the residue was extracted with methylene chloride. The organic layer was dried over magnesium sulfate and magnesium sulfate was filtered off, and then the filtrate was evaporated under reduced pressure. The residue was purified by silica gel column chromatography eluting with a mixed solvent of n-hexane-ethyl acetate (from 0% to 7% gradient elution) to give 5-bromo-2-(7-methoxyheptyloxy)-1,3-dimethylbenzene (3.34 g) as a colorless oil.

1. temperaturethe solution was refluxed for 8 hours
2. temperatureAfter cooling
3. customthe reaction mixture was evaporated under reduced pressure
4. extractionthe residue was extracted with methylene chloride
5. dry with materialThe organic layer was dried over magnesium sulfate and magnesium sulfate
6. filtrationwas filtered off
7. customthe filtrate was evaporated under reduced pressure
8. customThe residue was purified by silica gel column chromatography
9. washeluting with a mixed solvent of n-hexane-ethyl acetate (from 0% to 7% gradient elution)