HRID493378

反应详情

EQUATION

反应方程式

HRID 493378 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. additionis added at 23° C. to a solution
  2. temperatureis maintained for 30 minutes
  3. stirringThe reaction medium is stirred for one hour at 23° C.
  4. extractionextraction
  5. washthe organic phase is washed with a saturated sodium chloride solution
  6. dry with materialdried over sodium sulphate
  7. customthe solvent is evaporated off
  8. customThe residue obtained
  9. customthen purified by chromatography on a Biotage-type silica column (eluent: ethyl acetate-heptane: 6-1)
  10. customAn orange-coloured oil is obtained