HRID1824452

反应详情

EQUATION

反应方程式

HRID 1824452 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4-Benzyl-1-methyl-2-oxo-3-phenylpiperazine (15 g, 0.535 moles) was dissolved in acetic acid (120 ml) and added 5% palladium-carbon (50% wet, 1.5 g). Reaction mass was hydrogenated at 100 psi. After completion of the reaction, reaction mixture was filtered and acetic acid was distilled under reduced pressure. Residue was dissolved in DM water (75 ml). pH was adjusted to 11.0–12.0 with 50% aqueous sodium hydroxide solution. The product was extracted with methylene chloride (2×75 ml) and washed with DM water (75 ml). The methylene chloride layer was concentrated under reduced pressure to obtain 10.1 g of 1-methyl-2-oxo-3-phenylpiperazine.

WORKUP

后处理

  1. customReaction mass
  2. customAfter completion of the reaction, reaction mixture
  3. filtrationwas filtered
  4. distillationacetic acid was distilled under reduced pressure
  5. dissolutionResidue was dissolved in DM water (75 ml)
  6. extractionThe product was extracted with methylene chloride (2×75 ml)
  7. washwashed with DM water (75 ml)
  8. concentrationThe methylene chloride layer was concentrated under reduced pressure