反应详情

In 200 ml of anhydrous tetrahydrofuran were dissolved 30 g of 2',4',6'-trihydroxyacetophenone and 115.0 g of N,N-diisopropylethylamine, and 50.2 g of chloromethyl methyl ether was gradually added to the solution under ice cooling over a period of 20 minutes and the reaction mixture was stirred under ice cooling for 1 hour and at room temperature for 4 hours to effect reaction. After the reaction, the reaction mixture was extracted with 3 l of ether, and the ether layer was washed with water (500 ml×3 times), shaken with a saturated aqueous solution of sodium chloride (300 ml×2 times), dried with anhydrous sodium sulfate, and filtered. The solvent was removed from the filtrate by distillation and the obtained residue was recrystallized from a mixed solvent of methanol and water to obtain 18.9 g (yield=41.4%) of 2'-hydroxy-4',6'-bis(methoxyacetophenone in the form of a colorless prism.

1. additionwas gradually added to the solution under ice cooling over a period of 20 minutes
2. customreaction
3. customAfter the reaction
4. extractionthe reaction mixture was extracted with 3 l of ether
5. washthe ether layer was washed with water (500 ml×3 times)
6. stirringshaken with a saturated aqueous solution of sodium chloride (300 ml×2 times)
7. dry with materialdried with anhydrous sodium sulfate
8. filtrationfiltered
9. customThe solvent was removed from the filtrate by distillation
10. customthe obtained residue was recrystallized from a mixed solvent of methanol and water