반응 #4009

ord-c5c4f3d95a07449791cf3a5bbb4138ec

반응 조건

온도
50°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도After this time, the solution was cooled
  2. 2
    기타evaporated in vacuo
  3. 3
    기타The residue was partitioned between ethyl acetate and water
  4. 4
    기타the organic phase was separated
  5. 5
    세척washed three times with water
  6. 6
    건조then dried (MgSO4)
  7. 7
    기타Evaporation of the solvent
  8. 8
    기타gave the crude product which
  9. 9
    기타was purified by chromatography on silica (Merck Kieselgel 60)
  10. 10
    세척eluted with ether

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04723006uspto-grants-1988_02