HRID1287264

反应详情

EQUATION

反应方程式

HRID 1287264 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

14.5 g of N-[4-(β-<2-methoxy-5-methyl-benzamido>-ethyl)-benzenesulfonyl]-N'-phenyl-thiourea were dissolved in 50 ml of dioxane. After addition of 6 g of cyclopentyl-methylamine, the whole was heated for 2 hours to the boiling temperature under reflux. After having removed the dioxane by distillation, the residue was dissolved in 1% aqueous ammonia. The solution was filtered through charcoal and acidified with dilute hydrochloric acid. The N-[4-(β-<2-methoxy-5-methyl-benzamido>-ethyl)-benzenesulfonyl]-N'-cyclopentyl-methyl-thiourea so obtained was found to melt, after recrystallization from methanol, at 152° - 154° C.

WORKUP

后处理

  1. temperaturethe whole was heated for 2 hours to the boiling temperature
  2. temperatureunder reflux
  3. customAfter having removed the dioxane
  4. distillationby distillation
  5. dissolutionthe residue was dissolved in 1% aqueous ammonia
  6. filtrationThe solution was filtered through charcoal