HRID2198509

反应详情

EQUATION

反应方程式

HRID 2198509 的结构方程式

PROCEDURE

实验过程

50 ml abs. triethylamine, 50 ml abs. pyridine, 17.3 g (0.1 mol) 4-hydroxybenzamidine-hydrochloride and 11 g (0.1 mol) α-cyano-β-dimethylamino-acroleine are heated upon stirring for 6 hours to 80° C. Dark brown colored reaction mixture is poured on ice/concentrated H2SO4 (500 g/50 ml), the precipitate is removed by suction, washed thoroughly with water and recrystallized from methanol/activated carbon. The yield is 12.8 g (65% of the theoretical value). m.p.: 160-262 (sublimed).

WORKUP

后处理

  1. additionDark brown colored reaction mixture is poured on ice/concentrated H2SO4 (500 g/50 ml)
  2. customthe precipitate is removed by suction
  3. washwashed thoroughly with water
  4. customrecrystallized from methanol/activated carbon