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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
Ethyl benzoylacetate (2 mmol) and 4-methoxyphenylpiperazine (2 mmol) were dissolved in toluene, and refluxed for 24 hours. The resulting mixture was concentrated under a reduced pressure to obtain a crude compound, and the crude compound was dissolved in methanol, and cooled to 0° C. Then, sodium borohydride (2 mmol) was added dropwise to the resulting mixture. The mixture was stirred at a room temperature for 2 hours, concentrated under a reduced pressure, diluted with water, and then extracted several times with ethyl acetate to obtain an organic phase. The prepared organic phase was dried over magnesium sulfate, filtered, and then concentrated under a reduced pressure. The resulting pellet was purified with column chromatography (hexane:ethyl acetate=1:1) to obtain a compound. The prepared compound was dissolved in tetrahydrofuran (8 mL), and 1,1′-carbodiimidazole (4 mmol) was added to the resulting mixture. Then, the resulting mixture was stirred at a room temperature for 1 hour, and excessive dimethylamine was added to the reaction mixture. The resulting reaction mixture was stirred at a room temperature for 1 hour. The reaction mixture was diluted with water, and extracted several times with ethyl acetate to obtain an organic phase. The prepared organic phase was dried over magnesium sulfate, filtered, and then concentrated under a reduced pressure. The resulting pellet was purified with column chromatography (ethyl acetate) to obtain a title compound.
WORKUP
后处理
- temperaturerefluxed for 24 hours
- concentrationThe resulting mixture was concentrated under a reduced pressure
- customto obtain a crude compound
- concentrationconcentrated under a reduced pressure
- additiondiluted with water
- extractionextracted several times with ethyl acetate
- customto obtain an organic phase
- dry with materialThe prepared organic phase was dried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated under a reduced pressure
- customThe resulting pellet was purified with column chromatography (hexane:ethyl acetate=1:1)
- customto obtain a compound
- stirringThen, the resulting mixture was stirred at a room temperature for 1 hour
- customThe resulting reaction mixture
- stirringwas stirred at a room temperature for 1 hour
- extractionextracted several times with ethyl acetate
- customto obtain an organic phase
- dry with materialThe prepared organic phase was dried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated under a reduced pressure
- customThe resulting pellet was purified with column chromatography (ethyl acetate)