반응 #4786

ord-875c847cb5274fd89a51931bb3c68eed

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was refluxed for 6 hours
  2. 2
    여과After filtering off the insolubles
  3. 3
    workup.ADDITIONthe filtrate was poured into a suspension of chloroform (200 ml) and water (300 ml)
  4. 4
    기타The organic layer was separated
  5. 5
    세척washed with aqueous sodium chloride
  6. 6
    건조dried over magnesium sulfate
  7. 7
    기타The solvent was evaporated in vacuo
  8. 8
    기타the resulting crystals were recrystallized from ethanol

실험 절차

A suspension of 6-methyl-4-(3-nitrophenyl)-5-phthalimidomethyl-2-phenylpyrimidine (6.9 g) and hydrazine monohydrate (0.8 g) in ethanol (140 ml) was refluxed for 6 hours. After filtering off the insolubles, the filtrate was poured into a suspension of chloroform (200 ml) and water (300 ml) under stirring. The organic layer was separated, washed with aqueous sodium chloride and dried over magnesium sulfate. The solvent was evaporated in vacuo and the resulting crystals were recrystallized from ethanol to give 5-aminomethyl-6-methyl-4-(3-nitrophenyl)-2-phenylpyrimidine (1.12 g).

출처

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