反应详情

温度

45 °C

11.5 g of 2-methoxymethyloxy-4,5,6-trimethoxyphenol prepared in Referential Example 12 and 23.0 g of potassium carbonate were suspended in 100 ml of DMF. The suspension was heated at 45° C. while stirring, and 5.2 ml of iodomethane was dropwise added thereto. After the completion of the dropwise addition, the mixture was heated for 30 min, cooled and separated by filtration. 1 l of water was added to the mother liquor, and the mixture was extracted with ethyl acetate. The organic phase was washed with water and dried over anhydrous magnesium sulfate, and the solvent was distilled off. The residue was purified by silica gel column chromatography (eluent; n-hexane:ethyl acetate=85:15) to prepare 6.2 g of the product compound as a colorless oleaginous substance.

1. additionAfter the completion of the dropwise addition
2. temperaturethe mixture was heated for 30 min
3. temperaturecooled
4. customseparated by filtration
5. addition1 l of water was added to the mother liquor
6. extractionthe mixture was extracted with ethyl acetate
7. washThe organic phase was washed with water
8. dry with materialdried over anhydrous magnesium sulfate
9. distillationthe solvent was distilled off
10. customThe residue was purified by silica gel column chromatography (eluent; n-hexane:ethyl acetate=85:15)
11. customto prepare 6.2 g of the product compound as a colorless oleaginous substance