HRID394450

反应详情

EQUATION

反应方程式

HRID 394450 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 11.48 g (64,1 mmol) of 4,5-dichloro-2-methyl-3(2H)-pyridazinone and 31.84 g (193.0 mmol) of 3-(N-benzylamino)propanol in 250 ml of water is boiled for 25 hours while stirring. The mixture is cooled, its pH is set with concentrated hydrochloric acid to 3 and it is extracted with 2×400 ml of ethyl acetate. The organic phase is dried and evaporated, 10 ml of ethyl acetate are added to the evaporation residue, then it is left to stand overnight at −10° C. The precipitated crystals are filtered and washed with ethyl acetate and then with diethyl ether. In this way 10.60 g (54%) of the title compound are obtained with a melting point of 94-95° C.

WORKUP

后处理

  1. temperatureThe mixture is cooled
  2. extractionis extracted with 2×400 ml of ethyl acetate
  3. customThe organic phase is dried
  4. customevaporated
  5. addition10 ml of ethyl acetate are added to the evaporation residue
  6. waitit is left
  7. filtrationThe precipitated crystals are filtered
  8. washwashed with ethyl acetate