HRID1589715

反应详情

EQUATION

反应方程式

HRID 1589715 的结构方程式

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A mixture containing 11.85 g (0.035 mol) of methyl 2-[4-(5-trifluoromethyl-2-pyridyloxy)phenoxy]-propionate and 11.5 g (0.2 mol) of allylamine is boiled under reflux (about 60° C.) for 10 hours. (The reaction is followed by gas chromatography.) Thereafter, the excess of allylamine is distilled off and the residue is dissolved in benzene. After washing the solution cooled down with 5% aqueous hydrochloric acid and then with saturated sodium chloride solution, the organic phase is dried over anhydrous magnesium sulfate and evaporated. The crude product is recrystallized from petroleum ether (b.p. 120° C.) containing a small amount of toluene.

WORKUP

后处理

  1. distillation) Thereafter, the excess of allylamine is distilled off
  2. dissolutionthe residue is dissolved in benzene
  3. washAfter washing the solution
  4. temperaturecooled down with 5% aqueous hydrochloric acid
  5. dry with materialwith saturated sodium chloride solution, the organic phase is dried over anhydrous magnesium sulfate
  6. customevaporated
  7. customThe crude product is recrystallized from petroleum ether (b.p. 120° C.)
  8. additioncontaining a small amount of toluene