HRID1380221

反应详情

EQUATION

反应方程式

HRID 1380221 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a sodium methylate solution under agitation obtained by dissolving Na (2.8 g, 0.12 mol) in anhydrous methanol (20 c.c.) was added 4-fluorobenzamidine hydrochloride (10.5 g, 0.06 mol), followed by adding α-propyl-β-dimethylaminoacrolein (9.2 g, 0.06 mol), thereafter refluxing on heating for 3 hours with stirring, distilling off methanol under the atmospheric pressure after completion of the reaction, adding toluene (20cc) to the reaction residue to extract the resulting product, washing the extraction liquid with water, drying with anhydrous sodium sulfate, distilling off toluene and recrystallizing the remaining oily substance from ethanol (20 c.c.) to obtain the objective 5-propyl-2-(4-fluorophenyl)pyrimidine (7.0 g). Yield: 55%. M.P. 52.7° C.

WORKUP

后处理

  1. temperaturerefluxing
  2. temperatureon heating for 3 hours
  3. distillationdistilling off methanol under the atmospheric pressure
  4. customafter completion of the reaction
  5. extractionto extract the resulting product
  6. washwashing
  7. extractionthe extraction liquid with water
  8. dry with materialdrying with anhydrous sodium sulfate
  9. distillationdistilling off toluene
  10. customrecrystallizing the remaining oily substance from ethanol (20 c.c.)