反应详情

In 8 ml of chloroform were dissolved 85.7 mg of 3-acetyl-4-hydroxy-6-methyl-2H-pyran-2-one, 100 mg of 3-(2-methylthioethoxy)benzaldehyde and 30.3 mg of piperidine, and the solution was heated under refluxing for 13 hours while water was removed with a Soxhlet's extractor filled with a molecular sieve. After cooling to room temperature, the reaction mixture washed successively with 10% hydrochloric acid and an aqueous saturated sodium chloride solution, dried over anhydrous magnesium sulfate, and concentrated. Precipitated crystals were filtered, and this was subjected to silica gel column chromatography to obtain 10.1 mg of 4-piperidino-3-[3-[3-(2-methylthioethoxy)phenyl]-1-oxo-2-propenyl]-6-methyl-2H-pyran-2-one [Compound No. (14b)] as a pale yellow crystal.

1. temperaturethe solution was heated
2. customwas removed with a Soxhlet's extractor
3. additionfilled with a molecular sieve
4. washthe reaction mixture washed successively with 10% hydrochloric acid
5. dry with materialan aqueous saturated sodium chloride solution, dried over anhydrous magnesium sulfate
6. concentrationconcentrated
7. customPrecipitated crystals
8. filtrationwere filtered