HRID465944

反应详情

EQUATION

反应方程式

HRID 465944 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

To a solution of 1.57 g of 3-chloro-1-propanesulfonamide in 20 ml of methanol was added 20ml of 2N-potassium hydrogensulfide-ethanol solution, followed by heating at 70° C. for 50 minutes. Then, 1.48 g of 28% sodium methoxide-methanol solution and 1.32g of 3,6-dichloroimidazo[1,2-b]pyridazine were added to the reaction mixture and refluxed at 100° C. for 3 hours. The mixture was concentrated under reduced pressure, and to the residue was added 20 ml of water, which was adjusted to pH 7.0 with 1N-hydrochloric acid. The precipitated crystals were collected by filtration and recrystallized from methanol and ethyl ether to obtain 1.12 g of the title compound.

WORKUP

后处理

  1. temperaturerefluxed at 100° C. for 3 hours
  2. concentrationThe mixture was concentrated under reduced pressure
  3. additionto the residue was added 20 ml of water, which
  4. filtrationThe precipitated crystals were collected by filtration
  5. customrecrystallized from methanol and ethyl ether