반응 #2401

ord-c45d1e41cd734870bba0fc8cf09b8c4c

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타is reacted at 70° C. for two hours
  2. 2
    기타reacted at 90° C. for five hours
  3. 3
    추출extracted with ethyl acetate
  4. 4
    세척The ethyl acetate layer is washed
  5. 5
    기타dried
  6. 6
    기타evaporated
  7. 7
    기타to remove the solvent
  8. 8
    기타The residue is crystallized from hexane/ethyl acetate

실험 절차

A mixture of 6-chloro-5-(4-methylphenyl)pyrimidin-4-amine (500 mg), ethylene glycol (10 ml) and sodium hydride (60% dispersion-type, 0.46 g) is reacted at 70° C. for two hours, and reacted at 90° C. for five hours. The mixture is treated with saturated aqueous ammonium chloride solution, and extracted with ethyl acetate. The ethyl acetate layer is washed, dried, and evaporated to remove the solvent. The residue is crystallized from hexane/ethyl acetate to give 2-{6-amino-5-(4-methylphenyl)pyrimidin-4-yloxy}-ethanol (422 mg).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05728706uspto-grants-1998_03