HRID552035

反应详情

EQUATION

反应方程式

HRID 552035 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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, 7.7 g (0.0632 mol) of allyl bromide, 21 g (0.152 mol) of potassium carbonate and 200 mL of acetone. The mixture was refluxed with stirring overnight at which time it was allowed to cool, diluted with 200 mL of ethyl ether and filtered through a bed of Celite/activated charcoal. 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 yield 11 g of 2,2-dimethyl-5-allyl-1,3-dioxane-4,6-dione compound as shown in Formula (IV)) as a clear, colorless oil.

WORKUP

后处理

  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/activated charcoal
  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