HRID1169096
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
0.705 g of 4-(diphenylmethoxy)-1-piperidinepentanamine and 0.309 g of 6-chloro[1,2,4]triazolo[1,5-b]pyridazine were stirred at 135-140° C. for 1.5 hours. After cooling, aqueous sodium bicarbonate was added, followed by extraction with ethyl acetate; the extract was washed with saline, dried over sodium sulfate and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography and eluted with ethyl acetate:methanol:triethylamine (95:5:1). The desired fraction was collected, recrystallized from ethyl ether and dried to yield 0.629 g of the title compound.
WORKUP
后处理
- temperatureAfter cooling
- extractionfollowed by extraction with ethyl acetate
- washthe extract was washed with saline
- dry with materialdried over sodium sulfate
- concentrationconcentrated under reduced pressure
- washeluted with ethyl acetate:methanol:triethylamine (95:5:1)
- customThe desired fraction was collected
- customrecrystallized from ethyl ether
- customdried