HRID324906

反应详情

EQUATION

反应方程式

HRID 324906 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In a solvent mixture of 250 ml of acetic acid and 40 ml of ethyl acetate was dispersed 190 g of 1-benzylhydantoin and the mixture was refluxed under heating with stirring. To the mixture was added dropwise 164 g of bromine over a period of one hour, and the mixture was refluxed under heating for 30 minutes. The solvent was distilled off under a reduced pressure and the residue was allowed to stand for cooling. To the residue were added dropwise an aqueous sodium bicarbonate solution prepared by dissolving 53 g of sodium bicarbonate in 400 ml of water and then 200 ml of water. The reaction vessel was cooled with water and the crystals thus-deposited were collected by filtration, washed with water and dried to obtain 182 g of 5-hydroxy-1-benzylhydantoin as colorless crystals.

WORKUP

后处理

  1. temperaturethe mixture was refluxed
  2. temperatureunder heating
  3. temperaturethe mixture was refluxed
  4. temperatureunder heating for 30 minutes
  5. distillationThe solvent was distilled off under a reduced pressure
  6. temperaturefor cooling
  7. additionTo the residue were added dropwise an aqueous sodium bicarbonate solution
  8. customprepared
  9. filtrationthe crystals thus-deposited were collected by filtration
  10. washwashed with water
  11. customdried