反应详情

Combine methyl 3,5-dimethoxy-4-hydroxy-benzoate (2.12 g, 10 mmol) and dimethylformamide (50 mL). Cool in an ice bath. Add portionwise, sodium hydride (0.4 g, 16.7 mmol). after 2 hours, add iodoethane (4 mL, 50 mmol). Warm to ambient temperature. After 18 hours, dilute the reaction mixture with ethyl acetate and extract with water, 1M hydrochloric acid solution, a saturated sodium bicarbonate solution, and then brine. Dry the organic layer over MgSO4, filtered and evaporated in vacuo to give a residue. chromatograph the residue on silica gel eluting with 5% ethyl acetate/hexane to give methyl 3,5-dimethoxy-4-ethoxy-benzoate.

1. temperatureCool in an ice bath
2. additionAdd portionwise
3. waitAfter 18 hours
4. extractionextract with water, 1M hydrochloric acid solution
5. dry with materialDry the organic layer over MgSO4
6. filtrationfiltered
7. customevaporated in vacuo
8. customto give a residue