HRID1420573
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
A solution containing 13 g of 1-(2,5-dichlorobenzyl)-4-ethoxycarbonylpiperazine in 35 mL of 37% HCl was stirred for 40 h at reflux. Subsequently, 30 mL of water and 30 mL of EtOAc were added at room temperature, adjusting the pH to 11 via addition of 35% NaOH. The organic phase, which was dried on anhydrous sodium sulphate, was evaporated to dryness under vacuum. The crude was purified via flash chromatography (CHCl3 --MeOH 7:3) giving 4.46 g (50%) of the title compound.
WORKUP
后处理
- temperatureat reflux
- dry with materialThe organic phase, which was dried on anhydrous sodium sulphate
- customwas evaporated to dryness under vacuum
- customThe crude was purified via flash chromatography (CHCl3 --MeOH 7:3)