HRID64061
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- concentrationconcentrated on vacuum pump
- customThe mixture was quenched with sodium bicarbonate solution
- extractionextracted with ethyl acetate (3×150 ml)
- washThe combined organic layer was washed with water, brine
- dry with materialdried over sodium sulphate
- distillationThe solvent was distilled off
- customto give the product in 54.5% yield (0.6 g)
- custom159.1 [M+H]+ (rt: 0.102 min)