HRID465938

反应详情

EQUATION

反应方程式

HRID 465938 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6-Mercaptoimidazo[1,2-b]pyridazine (1.5 g) and 28 W/W % sodium methoxide-methanol solution (2.1 g) were stirred in 30 ml of methanol at 50° C. for 3 hours. The mixture was cooled to room temperature, 3.0 g of 3-aminosulfonyl-1-iodopropane were added and stirred at room temperature for 1.5 hours. The mixture was distilled to remove the solvent and the residue was subjected to a silica gel chromatography, which was eluted with successive 2 V/V % methanol-chloroform, 2.5 V/V % methanol-chloroform and 3.2 V/V % methanol-chloroform. The fractions containing the object compound were collected and concentrated. The precipitate was collected by filtration, thereby yielding 1.6 g of 6-(3-sulfamoyl-propylthio)imidazo [1,2-b]pyridazine.

WORKUP

后处理

  1. distillationThe mixture was distilled
  2. customto remove the solvent
  3. washwas eluted with successive 2 V/V % methanol-chloroform, 2.5 V/V % methanol-chloroform and 3.2 V/V % methanol-chloroform
  4. additionThe fractions containing the object compound
  5. customwere collected
  6. concentrationconcentrated
  7. filtrationThe precipitate was collected by filtration