HRID851782

反应详情

EQUATION

反应方程式

HRID 851782 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2 g. of the ethyl ester product from part (d) are dissolved in 100 ml. of ethanol. 0.5 g. of Lindlar catalyst are added and the reaction mixture is stirred for four hours at room temperature under two atmospheres of hydrogen. At intervals the reaction mixture is filtered. After completion of the slow absorption of hydrogen, the reaction solution is flooded with nitrogen and then heated to a boil. This mixture is filtered while hot and after cooling 1 g. of crude product is obtained from the filtrate. Recrystallization from water yields as white crystals purified 1-[(phenylmethylene)amino]-2,3-piperazinedione; m.p. 229°-231°.

WORKUP

后处理

  1. filtrationAt intervals the reaction mixture is filtered
  2. customAfter completion of the slow absorption of hydrogen
  3. temperatureheated to a boil
  4. filtrationThis mixture is filtered while hot and
  5. temperatureafter cooling 1 g
  6. customof crude product is obtained from the filtrate
  7. customRecrystallization from water
  8. customyields as white crystals
  9. custompurified 1-[(phenylmethylene)amino]-2,3-piperazinedione