HRID1057399

反应详情

EQUATION

反应方程式

HRID 1057399 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

(S)-(+)-2-Methylpiperazine (2.63 g), benzylbromide (3.12 ml) and potassium carbonate (5.4 g) were heated together in acetonitrile (120 ml) at 40° C. for 3 days. The mixture was evaporated to dryness in vacuo and the residue partitioned between aqueous sodium bicarbonate solution and ethyl acetate. The organic phase was separated, dried (magnesium sulphate) and evaporated to dryness in vacuo. The residue was purified by column chromatography over silica gel using gradient elution (95/510 to 92/7/1 dichloromethane/methanol/ammonium hydroxide) to afford the title compound as a solid, 1.12 g.

WORKUP

后处理

  1. customThe mixture was evaporated to dryness in vacuo
  2. customthe residue partitioned between aqueous sodium bicarbonate solution and ethyl acetate
  3. customThe organic phase was separated
  4. dry with materialdried (magnesium sulphate)
  5. customevaporated to dryness in vacuo
  6. customThe residue was purified by column chromatography over silica gel using gradient elution (95/510 to 92/7/1 dichloromethane/methanol/ammonium hydroxide)