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
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
500 ml of acetic acid was added to 57 g of 1-benzylhydantoin and, while maintaining at 80° C. with stirring, 50.3 g of bromine was dropwise added thereto. After completion of the dropwise addition, the solution was further stirred for 2 hours. The reaction solution was then cooled and, while cooling with ice, 56 g of ethylene glycol was added thereto. After stirring for 30 minutes, the solution was further stirred for 3 hours at room temperature. One liter of water was added to the reaction solution, followed by extraction with 500 ml of ethyl acetate. The extract was further washed twice with 500 ml of water. The thus obtained ethyl acetate solution was dried with sodium sulfate, concentrated, and purified by silica gel chromatography to obtain 52 g of 1-benzyl-5-(2-hydroxyethoxy)hydantoin. (Yield: 74%)
WORKUP
后处理
- additionAfter completion of the dropwise addition
- stirringthe solution was further stirred for 2 hours
- temperatureThe reaction solution was then cooled
- additionwas added
- stirringAfter stirring for 30 minutes
- stirringthe solution was further stirred for 3 hours at room temperature
- extractionfollowed by extraction with 500 ml of ethyl acetate
- washThe extract was further washed twice with 500 ml of water
- dry with materialThe thus obtained ethyl acetate solution was dried with sodium sulfate
- concentrationconcentrated
- custompurified by silica gel chromatography