HRID1195302

反应详情

EQUATION

反应方程式

HRID 1195302 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

15 ml of tetrahydrofuran and a catalytic amount of iodine were added to 340 mg of magnesium ribbon to obtain a mixture. 1.59 g of bromoethane was gradually added to the mixture in a stream of nitrogen in such a way that the reaction system was mildly refluxed. The resulting mixture was heated under reflux for 30 minutes and cooled, followed by the addition of a solution of 2 g of 5-acetyl-1,3-benzodioxole in tetrahydrofuran. The obtained mixture was stirred at a room temperature for 20 minutes, followed by the addition of a saturated aqueous solution of ammonium chloride and water. The obtained mixture was extracted with ethyl acetate. The organic layer was washed with a saturated aqueous solution of common salt, dried over anhydrous magnesium sulfate and filtered. The filtrate was distilled to remove the solvent. 2.27 g of the title compound was obtained as a crude oil.

WORKUP

后处理

  1. customto obtain a mixture
  2. temperaturewas mildly refluxed
  3. temperatureThe resulting mixture was heated
  4. temperatureunder reflux for 30 minutes
  5. temperaturecooled
  6. extractionThe obtained mixture was extracted with ethyl acetate
  7. washThe organic layer was washed with a saturated aqueous solution of common salt
  8. dry with materialdried over anhydrous magnesium sulfate
  9. filtrationfiltered
  10. distillationThe filtrate was distilled
  11. customto remove the solvent