HRID1584768

反应详情

EQUATION

反应方程式

HRID 1584768 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1,4-Diacetyl-2,5-piperazinedione (described by Marcuccio and Elix in Aust. J. Chem, 1984, 37, 1791) (25.0 g, 126 mmol) was treated at 130° C. in DMF (200 ml) with triethylamine (17.6 ml, 126 mmol) and benzaldehyde (13.0 ml, 126 mmol). After 4 hours the mixture was cooled to room temperature and poured into EtOAc (1000 ml) and washed 3 times with brine. Any solid formed at this stage was filtered off. The filtrate was dried (MgSO4) and the solvent removed in vacuo. The residue was recrystallised from EtOAc:Hexane to give 11.78 g (38%) of 1-acetyl-3-benzylidene-2,5-piperazinedione.

WORKUP

后处理

  1. washwashed 3 times with brine
  2. customAny solid formed at this stage
  3. filtrationwas filtered off
  4. dry with materialThe filtrate was dried (MgSO4)
  5. customthe solvent removed in vacuo
  6. customThe residue was recrystallised from EtOAc