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
0.341 g of 6-chloro[1,2,4]triazolo[4,3-b]pyridazin-3(2H)-one and 0.669 g of chlorotriphenylmethane were dissolved in 5 ml of N,N-dimethylformamide; 0.414 ml of N-ethyldiisopropylamine was added, followed by stirring at room temperature for 2 days. After water was added, the reaction mixture was extracted with ethyl acetate; the extract was washed with saline and dried over magnesium sulfate. After concentration under reduced pressure, the residue was subjected to silica gel column chromatography and eluted with hexane-ethyl acetate (2:1). The desired fraction was collected and concentrated; the crystal obtained was collected by filtration, washed with diethyl ether, and dried, to yield 0.591 g of the title compound.
WORKUP
后处理
- extractionthe reaction mixture was extracted with ethyl acetate
- washthe extract was washed with saline
- dry with materialdried over magnesium sulfate
- concentrationAfter concentration under reduced pressure
- washeluted with hexane-ethyl acetate (2:1)
- customThe desired fraction was collected
- concentrationconcentrated
- customthe crystal obtained
- filtrationwas collected by filtration
- washwashed with diethyl ether
- customdried