反应 #4392

ord-022e022fa6a34c4ca3ba0dec5c804a5d

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他evaporated in vacuo
  2. 2
    workup.ADDITIONTo the residue was added aqueous sodium bicarbonate solution
  3. 3
    萃取the mixture was extracted with methylene chloride
  4. 4
    洗涤The extract was washed with brine
  5. 5
    干燥dried over magnesium sulfate
  6. 6
    其他evaporated in vacuo
  7. 7
    其他The oily residue was purified by column chromatography on silica gel (40 g) with a mixture of methylene chloride and ethyl acetate (10:1) as an eluent

实验过程

A solution of 2-amino-3-(2-methylbenzylamino)pyridine (3.25 g) and chloroacetone (1.26 ml) in ethanol (65 ml) was refluxed for 18 hours and then evaporated in vacuo. To the residue was added aqueous sodium bicarbonate solution and the mixture was extracted with methylene chloride. The extract was washed with brine, dried over magnesium sulfate, and evaporated in vacuo. The oily residue was purified by column chromatography on silica gel (40 g) with a mixture of methylene chloride and ethyl acetate (10:1) as an eluent to give 8-(2-methylbenzylamino)-2-methylimidazo[1,2-a]pyridine (1.80 g).

来源

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