HRID1164764

反应详情

EQUATION

反应方程式

HRID 1164764 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To 4,6-dichloro-5-methoxy-2-(4-octylphenyl)pyrimidine (74.2 g, 0.202 mol) were added ethanol (310 ml), water (15.5 ml), 5% Pd-activated carbon (5.7 g) and triethylamine (61.3 g, 0.606 mol), followed by agitating the mixture at about 40° C. in hydrogen current, filtering off the Pd-activated carbon adding toluene, sufficiently washing the mixture with 2N-NaOH aqueous solution, further washing it with water, distilling off toluene and recrystallizing the residue from ethanol (70 ml) to obtain 5-methoxy-2-(4-octylphenyl)pyrimidine in the form of colorless acicular crystals (54.9 g) having a m.p. of 40.1-41.8° C.

WORKUP

后处理

  1. filtrationfiltering off the Pd-activated carbon
  2. additionadding toluene
  3. washsufficiently washing the mixture with 2N-NaOH aqueous solution
  4. washfurther washing it with water
  5. distillationdistilling off toluene
  6. customrecrystallizing the residue from ethanol (70 ml)