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
PROCEDURE
实验过程
3-amino-6-mercaptopyridazine (0.5 g), 3-chloromethyl-4-propyl-4H-1,2,4-triazole hydrochloride (0.57 g) and potassium carbonate (0.8 g) were added to N,N-dimethylformamide (5 ml), and the mixture was stirred for 4.5 hours at room temperature. The solvent was distilled off, and to the residue was added water, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated brine, and dried over anhydrous magnesium sulfate, and then, the solvent was distilled off. The residue was purified by basic silica gel column chromatography (elution solvent: methanol/ethyl acetate), to give 3-amino-6-[(4-propyl-1H-1,2,4-triazol-3-yl)methylthio]pyridazine (0.62 g) as colorless crystals.
WORKUP
后处理
- distillationThe solvent was distilled off
- additionto the residue was added water
- extractionthe mixture was extracted with ethyl acetate
- washThe organic layer was washed with water and saturated brine
- dry with materialdried over anhydrous magnesium sulfate
- distillationthe solvent was distilled off
- customThe residue was purified by basic silica gel column chromatography (elution solvent: methanol/ethyl acetate)