HRID703929
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe solution was heated
- temperatureunder reflux for 6 hours
- temperatureAfter cooling
- filtrationthe insoluble substance was filtered off
- distillationethanol was distilled away
- dissolutionThe residue was dissolved in ethyl acetate
- washwashed with 5% sodium carbonate and brine
- dry with materialdried over anhydrous sodium sulfate
- distillationEthyl acetate was distilled away
- customthe residue was recrystallized from hexane