HRID1608210

反应详情

EQUATION

反应方程式

HRID 1608210 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-acetylaminomethylmorpholine (7.0 g), 4-fluorobenzyl chloride (12 g), potassium carbonate (56 g), potassium iodide (1 g), and methyl ethyl ketone (100 ml) is refluxed with stirring for 17 hours. The reaction mixture is filtered and the filtrate is concentrated under reduced pressure. The residue is diluted with water and extracted with chloroform. The organic layer is separated, washed successively with water and saturated aqueous sodium chloride solution, and dried over magnesium sulfate. The solvent is distilled off under reduced pressure, and the residue is recrystallized from toluene to give the title compound (9.3 g), mp 120°-122° C.

WORKUP

后处理

  1. temperatureis refluxed
  2. filtrationThe reaction mixture is filtered
  3. concentrationthe filtrate is concentrated under reduced pressure
  4. additionThe residue is diluted with water
  5. extractionextracted with chloroform
  6. customThe organic layer is separated
  7. washwashed successively with water and saturated aqueous sodium chloride solution
  8. dry with materialdried over magnesium sulfate
  9. distillationThe solvent is distilled off under reduced pressure
  10. customthe residue is recrystallized from toluene