HRID1638946

反应详情

EQUATION

反应方程式

HRID 1638946 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
  4. washNaOH aqueous solution, further washing it with water
  5. distillationdistilling off toluene
  6. customrecrystallizing the residue from ethanol (70 ml)