HRID2254555

反应详情

EQUATION

反应方程式

HRID 2254555 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1.8 g 3-chloro-6-(3-methoxy-4-n-propoxyphenyl)pyridazine, 0.8 g sodium cyanamide and 3.6 g tetrabutylammonium chloride are boiled under reflux in 30 ml dry toluene for 5 hours. The reaction mixture is then evaporated in vacuo and the residue is boiled up briefly with 200 ml 2 N sodium hydrogen sulphate solution, while stirring thoroughly, the reaction product precipitating as a fine crystalline precipitate. The precipitate is filtered off with suction, washed with water and dried in vacuo. For purification, it is boiled up briefly with 50 ml isopropanol, filtered off with suction and dried in vacuo. This gives 1.5 g (83.3%) of the title compound of m.p. 187° C.

WORKUP

后处理

  1. customThe reaction mixture is then evaporated in vacuo
  2. customthe reaction product precipitating as a fine crystalline precipitate
  3. filtrationThe precipitate is filtered off with suction
  4. washwashed with water
  5. customdried in vacuo
  6. customFor purification, it
  7. filtrationfiltered off with suction
  8. customdried in vacuo