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
Sodium hydride (3.18 g; 0.0795 mol of a powder dispersed at 60%) is added at 23° C. to a solution containing 4-(2-hydroxyethyl)morpholine (9.40 g, 0.072 mol) in dimethylformamide (60 ml). Stirring is maintained for 30 minutes then the compound 4-fluoroacetophenone (5 g, 0.0362 mol) is added. The reaction medium is stirred for one hour at 23° C. then cooled down to 0° C. and water is added. After the addition of ethyl acetate then extraction, the organic phase is washed with a saturated sodium chloride solution, dried over sodium sulphate then the solvent is evaporated off. The residue obtained is adsorbed on silica then purified by chromatography on a Biotage-type silica column (eluent: ethyl acetate-heptane: 6-1). An orange-coloured oil is obtained.
WORKUP
后处理
- additionis added at 23° C. to a solution
- temperatureis maintained for 30 minutes
- stirringThe reaction medium is stirred for one hour at 23° C.
- extractionextraction
- washthe organic phase is washed with a saturated sodium chloride solution
- dry with materialdried over sodium sulphate
- customthe solvent is evaporated off
- customThe residue obtained
- customthen purified by chromatography on a Biotage-type silica column (eluent: ethyl acetate-heptane: 6-1)
- customAn orange-coloured oil is obtained