反应详情

To a solution of titanium (IV) chloride (11.1 g) in THF (50 mL) was added dropwise a solution of 2,2-dimethyl-1,3-dioxane-4,6-dione (4.26 g) and 3-hydroxy-4-methoxybenzaldehyde (3.00 g) in THF (50 mL) at 0° C., and then a solution of pyridine (4.00 g) in THF (20 mL) was added dropwise. The reaction mixture was stirred for 1 hr, and water was added to the reaction mixture. The reaction mixture was extracted with ethyl acetate, and the extract was washed with 1N hydrochloric acid and saturated brine. The organic layer was dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure to give the title compound (3.50 g) as a yellow solid. This compound was used for the next step without further purification.

1. extractionThe reaction mixture was extracted with ethyl acetate
2. washthe extract was washed with 1N hydrochloric acid and saturated brine
3. dry with materialThe organic layer was dried over anhydrous sodium sulfate
4. customThe solvent was evaporated under reduced pressure