HRID1886307

反应详情

EQUATION

反应方程式

HRID 1886307 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionAfter completion of the dropwise addition
  2. stirringthe solution was further stirred for 2 hours
  3. temperatureThe reaction solution was then cooled
  4. additionwas added
  5. stirringAfter stirring for 30 minutes
  6. stirringthe solution was further stirred for 3 hours at room temperature
  7. extractionfollowed by extraction with 500 ml of ethyl acetate
  8. washThe extract was further washed twice with 500 ml of water
  9. dry with materialThe thus obtained ethyl acetate solution was dried with sodium sulfate
  10. concentrationconcentrated
  11. custompurified by silica gel chromatography