HRID64061

反应详情

EQUATION

反应方程式

HRID 64061 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The solution of methyl 2-(4-ethylpiperazin-1-yl)acetate (1.3 g, 6.50 mmol, 1.0 eq) in 8 N HCl was stirred at 95° C. for 16 h and concentrated on vacuum pump. The mixture was quenched with sodium bicarbonate solution and extracted with ethyl acetate (3×150 ml). The combined organic layer was washed with water, brine and dried over sodium sulphate. The solvent was distilled off to give the product in 54.5% yield (0.6 g). LC-MS (ESI): Calculated mass: 158.0; Observed mass: 159.1 [M+H]+ (rt: 0.102 min).

WORKUP

后处理

  1. concentrationconcentrated on vacuum pump
  2. customThe mixture was quenched with sodium bicarbonate solution
  3. extractionextracted with ethyl acetate (3×150 ml)
  4. washThe combined organic layer was washed with water, brine
  5. dry with materialdried over sodium sulphate
  6. distillationThe solvent was distilled off
  7. customto give the product in 54.5% yield (0.6 g)
  8. custom159.1 [M+H]+ (rt: 0.102 min)