HRID2426868

反应详情

EQUATION

反应方程式

HRID 2426868 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of 5-benzylhexahydropyrrolo[3,4-c]pyrrole-1-one, (7.2 g; 33 mmol) in absolute ethanol (100 ml) is placed in a 250 ml autoclave and palladium-on-charcoal at 5% (1.5 g) is then added. After having purged with nitrogen, the autoclave is placed under 56 bar of hydrogen at 70° C. for 16 hours. After returning to 20° C., the catalyst is filtered off and the filtrate is evaporated under reduced pressure. The compound obtained is taken up in acetonitrile (15 ml) at reflux, filtered, under hot conditions, through paper and then crystallized. After crystallization, the solid obtained is filtered off, washed with acetonitrile (3 ml) and then with diethyl ether (20 ml) and, finally, dried under reduced pressure at constant weight. Hexahydropyrrolo[3,4-c]pyrrole-1-one, (1.3 g; 31%) is isolated, the characteristics of which are as follows:

WORKUP

后处理

  1. additionis then added
  2. customAfter having purged with nitrogen
  3. customAfter returning to 20° C.
  4. filtrationthe catalyst is filtered off
  5. customthe filtrate is evaporated under reduced pressure
  6. customThe compound obtained
  7. temperatureat reflux
  8. filtrationfiltered, under hot conditions, through paper
  9. customcrystallized
  10. customAfter crystallization
  11. customthe solid obtained
  12. filtrationis filtered off
  13. washwashed with acetonitrile (3 ml)
  14. dry with materialwith diethyl ether (20 ml) and, finally, dried under reduced pressure at constant weight