HCID 69148098, compound → 1,6-dimethyl-2-Piperazinone

HRID 2114850Notes

Reaction equation

HRID 2114850 reaction equation
[CH3:1][CH:2]1[N:7]([CH3:8])[C:6](=[O:9])[CH2:5][N:4](C(OCC2C=CC=CC=2)=O)[CH2:3]1>CCO>[CH3:8][N:7]1[CH:2]([CH3:1])[CH2:3][NH:4][CH2:5][C:6]1=[O:9]

Participants

3

Procedure

A solution of benzyl 3,4-dimethyl-5-oxopiperazine-1-carboxylate (780 mg, 2.97 mmol) in EtOH was degassed and purged with nitrogen and treated with 10% palladium on carbon (78 mg). The mixture was degassed and purged with nitrogen again and placed under a balloon atmosphere of hydrogen. The reaction was stirred for 3 h at room temperature and filtered through a pad of Celite, washing with MeOH. The resulting filtrate was concentrated to an oil which was dissolved in toluene. The solution was again filtered through Celite, and the resulting filtrate was concentrated in vacuo to afford the product.

Workup

  1. custompurged with nitrogen
  2. additiontreated with 10% palladium on carbon (78 mg)
  3. customThe mixture was degassed
  4. custompurged with nitrogen again
  5. filtrationfiltered through a pad of Celite
  6. washwashing with MeOH
  7. concentrationThe resulting filtrate was concentrated to an oil which
  8. dissolutionwas dissolved in toluene
  9. filtrationThe solution was again filtered through Celite
  10. concentrationthe resulting filtrate was concentrated in vacuo
  11. customto afford the product

Sources & evidence

ORD record
ord-a4540ed4534a4dbe88ccd8680c7b7036
Source dataset
uspto-grants-2008_10
Patent number
US07435735B2

Reaction notes

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