HRID1732650

反应详情

EQUATION

反应方程式

HRID 1732650 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4-Acetyl-5,6-bis(p-chlorophenyl)-2H-pyridazin-3-one (20.0 g), potassium carbonate (9.0 g) and 30 ml of a toluene solution of N-(2-chloroethyl)dimethylamine (0.34 g/ml) and dimethylformamide (150 ml) were stirred at 80° C. for 18 hours. A second equivalent of the amine was added and heating continued for an additional four hours. The mixture was cooled, poured into water and the suspension extracted with ethyl acetate. The combined organic extracts were dried and evaporated in vacuo. Following purification by dry column silica gel chromatography and recrystallization, the title compound was obtained (63 percent yield), m.p. 149°-150° C.

WORKUP

后处理

  1. temperatureheating
  2. temperatureThe mixture was cooled
  3. extractionthe suspension extracted with ethyl acetate
  4. customThe combined organic extracts were dried
  5. customevaporated in vacuo
  6. custompurification
  7. customby dry
  8. customcolumn silica gel chromatography and recrystallization