HRID896584

反应详情

EQUATION

反应方程式

HRID 896584 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

5,5-Diphenylimidazolidine-2,4-dione (0.5 g) was dissolved in tetrahydrofuran (5 mL), and sodium hydride (60%, in oil) (87 mg) was added at 0° C. under ice-cooling. After stirred for 30 minutes, 2-furoyl chloride (235 mg) was added 0° C., and the mixture was stirred at room temperature for 2.5 hours. After water was added carefully, ethyl acetate (200 mL) was added, and the layers were separated. The resulting organic layer was washed with a saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was distilled off. Further purification by silica gel chromatography (hexane:ethyl acetate=2:1) afforded white powders. The resulting foam was recrystallized from IPE to obtain 273 mg of white crystals.

WORKUP

后处理

  1. temperaturecooling
  2. stirringthe mixture was stirred at room temperature for 2.5 hours
  3. customthe layers were separated
  4. washThe resulting organic layer was washed with a saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationthe solvent was distilled off
  7. customFurther purification by silica gel chromatography (hexane:ethyl acetate=2:1)
  8. customafforded white powders
  9. customThe resulting foam was recrystallized from IPE