HRID703929

反应详情

EQUATION

反应方程式

HRID 703929 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.7 g of potassium hydroxide was dissolved in 150 ml of ethanol. 5.1 g of 1-methylparabanic acid and 10 ml of ethyl bromoacetate were added thereto and the solution was heated under reflux for 6 hours. After cooling, the insoluble substance was filtered off and ethanol was distilled away. The residue was dissolved in ethyl acetate, washed with 5% sodium carbonate and brine, dried over anhydrous sodium sulfate, and passes through silica gel column. Ethyl acetate was distilled away and the residue was recrystallized from hexane to give 3.1 g of ethyl 1-methyl-2,4,5-trioxoimidazolidine-3-acetate (Compound 1).

WORKUP

后处理

  1. temperaturethe solution was heated
  2. temperatureunder reflux for 6 hours
  3. temperatureAfter cooling
  4. filtrationthe insoluble substance was filtered off
  5. distillationethanol was distilled away
  6. dissolutionThe residue was dissolved in ethyl acetate
  7. washwashed with 5% sodium carbonate and brine
  8. dry with materialdried over anhydrous sodium sulfate
  9. distillationEthyl acetate was distilled away
  10. customthe residue was recrystallized from hexane