反応 #4009

ord-c5c4f3d95a07449791cf3a5bbb4138ec

反応条件

温度
50°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

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

実験手順

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.

出典

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