反应 #4009

ord-c5c4f3d95a07449791cf3a5bbb4138ec

反应条件

温度
50°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度After this time, the solution was cooled
  2. 2
    其他evaporated in vacuo
  3. 3
    其他The residue was partitioned between ethyl acetate and water
  4. 4
    其他the organic phase was separated
  5. 5
    洗涤washed three times with water
  6. 6
    干燥then dried (MgSO4)
  7. 7
    其他Evaporation of the solvent
  8. 8
    其他gave the crude product which
  9. 9
    其他was purified by chromatography on silica (Merck Kieselgel 60)
  10. 10
    洗涤eluted with ether

实验过程

3,56 Parts of 2-amino-4-chloro-6-chloromethylpyrimidine and 2.24 parts of potassium t-butoxide were dissolved in 60 parts of n-butanol at room temperature then the solution was heated at 50° C. for 2 hours, with stirring. After this time, the solution was cooled and evaporated in vacuo. The residue was partitioned between ethyl acetate and water and the organic phase was separated and washed three times with water then dried (MgSO4). Evaporation of the solvent gave the crude product which was purified by chromatography on silica (Merck Kieselgel 60) eluted with ether to give 2-amino-4-n-butoxy-6-chloromethylpyrmidine as an oil.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04723006uspto-grants-1988_02