HRID1834904

反应详情

EQUATION

反应方程式

HRID 1834904 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

At about 20° C, 10.5 parts of triethylamine and subsequently 12.4 parts of methylmethoxycarbamoyl chloride are added to a suspension of 24.5 parts of 3-(3,5-dichlorophenyl)-hydantoin in 250 parts of dry tetrahydrofuran. After all has been added, the mixture is refluxed for 3 hours. After the mixture has been cooled to 20° C, the precipitated triethylamine hydrochloride is removed by suction filtration. The filtrate is concentrated. The residue is dissolved in a 1:1 mixture of n-pentane and ether, suction filtered, dried and recrystallized from toluene.

WORKUP

后处理

  1. additionAfter all has been added
  2. temperaturethe mixture is refluxed for 3 hours
  3. customthe precipitated triethylamine hydrochloride is removed by suction filtration
  4. concentrationThe filtrate is concentrated
  5. dissolutionThe residue is dissolved in a 1:1 mixture of n-pentane and ether, suction
  6. filtrationfiltered
  7. customdried
  8. customrecrystallized from toluene