반응 #4779

ord-f9e672f1e9b44c4186cfbb5036d7a208

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was refluxed for 6 hours
  2. 2
    기타After evaporating the solvent
  3. 3
    workup.DISSOLUTIONthe residue was dissolved in chloroform
  4. 4
    세척washed with saturated aqueous sodium chloride
  5. 5
    건조dried over magnesium sulfate
  6. 6
    기타The filtrate was evaporated under reduced pressure
  7. 7
    세척eluting with chloroform
  8. 8
    workup.ADDITIONThe fractions containing the object compound
  9. 9
    농축concentrated under reduced pressure
  10. 10
    기타The residue was recrystallized from diethyl ether

실험 절차

A mixture of 5-bromomethyl-6-methyl-4-(3-nitrophenyl)-2-phenylpyrimidine (1.5 g), N-methylpiperazine (1.17 g) in isopropyl alcohol (15 ml) was refluxed for 6 hours. After evaporating the solvent, the residue was dissolved in chloroform, washed with saturated aqueous sodium chloride and dried over magnesium sulfate. The filtrate was evaporated under reduced pressure, and the residue was subjected to column chromatography on alumina (100 g) eluting with chloroform. The fractions containing the object compound were combined and concentrated under reduced pressure. The residue was recrystallized from diethyl ether to give 6-methyl-5-(4-methylpiperazin-1-ylmethyl)-4-(3-nitrophenyl)-2-phenylpyrimidine. (0.30 g).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04727073uspto-grants-1988_02