HRID649811

反应详情

EQUATION

反应方程式

HRID 649811 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture comprising 1.94 g 1-ethoxycarbonylpiperazine and 3.45 g anhydrous potassium carbonate, in 20 mL of N,N-dimethylformamide, stirred at room temperature, under a nitrogen atmosphere, there was added 2.01 g of 2,5-dichlorobenzyl chloride. Then after 24 hr stirring at room temperature, this reaction mixture was poured into 200 mL of water, followed by extraction with ethyl acetate (3×100 mL). The obtained organic phase was dried over anhydrous sodium sulphate, followed by evaporation under vacuum. The obtained residue was then purified by flash chromatography (petroleum ether—ethyl acetate 85:15). The solvents were then evaporated off completely to give 2 g of Compound 14A (yield 63%).

WORKUP

后处理

  1. extractionfollowed by extraction with ethyl acetate (3×100 mL)
  2. dry with materialThe obtained organic phase was dried over anhydrous sodium sulphate
  3. customfollowed by evaporation under vacuum
  4. customThe obtained residue was then purified by flash chromatography (petroleum ether—ethyl acetate 85:15)
  5. customThe solvents were then evaporated off completely