反应 #4402

ord-b00092430ac54cc19a9bd1a0f1697fff

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度the mixture was heated at 90°-95° C.
  2. 2
    温度After being cooled
  3. 3
    过滤the resulting precipitate was collected by filtration
  4. 4
    workup.DISSOLUTIONdissolved in methylene chloride
  5. 5
    workup.ADDITIONThe solution was treated successively with silica gel (1 g) and activated charcoal
  6. 6
    其他evaporated in vacuo
  7. 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).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04725601uspto-grants-1988_02