HRID2164407

反应详情

EQUATION

反应方程式

HRID 2164407 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

15.3 g of 5-phenoxysulfonyl-2-ureidoaniline, 12 g of N,N'-bismethoxycarbonyl-S-methylisothiourea and 100 mg of p-toluenesulfonic acid in 80 ml of methanol and 80 ml of ethyl acetate are stirred under reflux for four hours. After cooling down, the solid is filtered off with suction and washed with ethyl acetate and diisopropyl ether. For recrystallization, the solid is dissolved in dimethylformamide at about 50° C., treated with active charcoal, filtered, ethyl acetate and diisopropyl ether are added and crystallization is allowed to occur, melting point 193° C., decomposition.

WORKUP

后处理

  1. temperatureunder reflux for four hours
  2. temperatureAfter cooling down
  3. filtrationthe solid is filtered off with suction
  4. washwashed with ethyl acetate and diisopropyl ether
  5. customFor recrystallization
  6. dissolutionthe solid is dissolved in dimethylformamide at about 50° C.
  7. additiontreated with active charcoal
  8. filtrationfiltered
  9. additionethyl acetate and diisopropyl ether are added
  10. customcrystallization