HRID493329

反应详情

EQUATION

反应方程式

HRID 493329 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To an ice cold (˜0° C.) suspension of cis-2,6-dimethylpiperazine (4.0 g, 35 mmol) in DMF (100 mL) was benzyl bromide (6.0 g, 35.0 mmol) added in portions under a period of 45 min and the reaction mixture was stirred at room temperature for 48 h. The solvent was evaporated from the suspension and the residue was dissolved in aqueous HCl and washed twice with CHCl3. The aqueous phase was made alkaline and extracted twice with CHCl3. The combined organic phases were washed with H2O and brine, dried (MgSO4), and concentrated to give 4.9 g (68%) of the title product as a colorless oil.

WORKUP

后处理

  1. additionadded in portions under a period of 45 min
  2. customThe solvent was evaporated from the suspension
  3. dissolutionthe residue was dissolved in aqueous HCl
  4. washwashed twice with CHCl3
  5. extractionextracted twice with CHCl3
  6. washThe combined organic phases were washed with H2O and brine
  7. dry with materialdried (MgSO4)
  8. concentrationconcentrated