反应详情

To a 500 mL 3-necked round bottomed flask equipped with a stir bar, thermowell, and a condenser connected to a nitrogen line was added 10.0 g (0.0632 mole) of 2,2,5-trimethyl-1,3-dioxane-4,6-dione, 10.6 g (0.0632 mol) of p-(chloromethyl)styrene, 35 g (0.2528 mol) of potassium carbonate and 200 mL of acetone. Approximately 1 g of phenothiazine was added as a stabilizer. The mixture was refluxed with stirring overnight at which time it was allowed to cool, diluted with 200 mL of ethyl acetate and filtered through a bed of Celite. The filtrate was washed with water and brine and dried overnight over anhydrous sodium sulfate. The suspension was filtered and the filtrate evaporated on a rotary evaporator to a light brown oil which spontaneously crystallized. The crystals were collected and washed with 35-65 petroleum ether to yield 3.5 g of 2,2-dimethyl-5-(4-vinylbenzyl)-1,3-dioxane-4,6-dione as shown by formula (III).

1. customTo a 500 mL 3-necked round bottomed flask equipped with a stir bar
2. customthermowell, and a condenser connected to a nitrogen line
3. temperatureThe mixture was refluxed
4. temperatureto cool
5. filtrationfiltered through a bed of Celite
6. washThe filtrate was washed with water and brine
7. dry with materialdried overnight over anhydrous sodium sulfate
8. filtrationThe suspension was filtered
9. customthe filtrate evaporated on a rotary evaporator to a light brown oil which
10. customspontaneously crystallized
11. customThe crystals were collected
12. washwashed with 35-65 petroleum ether