反应 #4402
ord-b00092430ac54cc19a9bd1a0f1697fff
反应方程式
反应物
试剂
反应条件
后处理
- 1温度the mixture was heated at 90°-95° C.
- 2温度After being cooled
- 3过滤the resulting precipitate was collected by filtration
- 4workup.DISSOLUTIONdissolved in methylene chloride
- 5workup.ADDITIONThe solution was treated successively with silica gel (1 g) and activated charcoal
- 6其他evaporated in vacuo
- 7其他The crystalline residue was recrystallized from a mixture of methylene chloride and n-hexane
实验过程
To a solution of sodium hydride (60% in mineral oil dispersion, 0.186 g) in 2-propynyl alcohol (8 ml) was added 8-(2-chlorobenzyloxy)-3-trimethylammoniomethyl-2-methylimidazo[1,2-a]pyridine iodide (2 g) and the mixture was heated at 90°-95° C. with stirring for 1 hour. After being cooled, the mixture was poured into ice-water and the resulting precipitate was collected by filtration and dissolved in methylene chloride. The solution was treated successively with silica gel (1 g) and activated charcoal and evaporated in vacuo. The crystalline residue was recrystallized from a mixture of methylene chloride and n-hexane to give 8-(2-chlorobenzyloxy)-3-(2-propynyloxymethyl)-2-methylimidazo[1,2-a]pyridine (0.9 g).