HRID1885537
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 150 °C
PROCEDURE
实验过程
6-Chloroimidazo[1,2-b]pyridazine (13.5 g), 28 W/W% sodium methoxide-methanol solution (17.5 g) and thioacetic acid (7.0 g) were dissolved in 70 ml of methanol and this solution was heated at 150° C. in a sealed tube for 6 hours. The reaction mixture was cooled to room temperature and distilled to remove the organic solvent. The residue was washed three times with chloroform (50 ml), and the insoluble material was extracted six times with 50 ml of chloroform-methanol (1:1) solution. The combined extracts were distilled to remove the organic solvent. The precipitated crystals were collected by filtration, thereby obtaining 6-mercaptoimidazo[1,2-b]pyridazine (3.7 g).
WORKUP
后处理
- temperatureThe reaction mixture was cooled to room temperature
- distillationdistilled
- customto remove the organic solvent
- washThe residue was washed three times with chloroform (50 ml)
- extractionthe insoluble material was extracted six times with 50 ml of chloroform-methanol (1:1) solution
- distillationThe combined extracts were distilled
- customto remove the organic solvent
- filtrationThe precipitated crystals were collected by filtration