Реакция #2401

ord-c45d1e41cd734870bba0fc8cf09b8c4c

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеis reacted at 70° C. for two hours
  2. 2
    Другоеreacted at 90° C. for five hours
  3. 3
    Экстракцияextracted with ethyl acetate
  4. 4
    ПромывкаThe ethyl acetate layer is washed
  5. 5
    Другоеdried
  6. 6
    Другоеevaporated
  7. 7
    Другоеto remove the solvent
  8. 8
    ДругоеThe residue is crystallized from hexane/ethyl acetate

Методика

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).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05728706uspto-grants-1998_03