HRID865376

反应详情

EQUATION

反应方程式

HRID 865376 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

Forty milliliters of ethyleneglycol monomethyl ether, 3.84 g of 5-(3-cyclohexene-1-yl)methylenehydantoin and 0.43 g of wet 10% palladium on carbon (moisture 50%) were placed in a reactor equipped with a mechanical stirrer and a reflux condenser, and the mixture was reduced while stirring at 50° C. under a hydrogen pressure of 3 kg/cm2. After 4 hours, the reaction mixture was heated to 90° C. and the resulting precipitate was dissolved, after which the palladium on carbon was removed by filtering the hot mixture. To the slurry obtained by concentrating the filtrate to about 20 ml was added 100 ml of water, by which were obtained white crystals which were then collected by filtration and washed with water, and then dried under reduced pressure at 60° C. overnight to obtain 3.50 g of 5-cyclohexylmethylhydantoin. The yield was 89.2%. The crude crystals were recrystallized from ethanol to obtain a pure product.

WORKUP

后处理

  1. customequipped with a mechanical stirrer and a reflux condenser
  2. temperaturethe reaction mixture was heated to 90° C.
  3. dissolutionthe resulting precipitate was dissolved
  4. customafter which the palladium on carbon was removed
  5. filtrationby filtering the hot mixture
  6. customTo the slurry obtained
  7. concentrationby concentrating the filtrate to about 20 ml
  8. additionwas added 100 ml of water
  9. customby which were obtained white crystals which
  10. filtrationwere then collected by filtration
  11. washwashed with water
  12. customdried under reduced pressure at 60° C. overnight