反応 #2401

ord-c45d1e41cd734870bba0fc8cf09b8c4c

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他is reacted at 70° C. for two hours
  2. 2
    その他reacted at 90° C. for five hours
  3. 3
    抽出extracted with ethyl acetate
  4. 4
    洗浄The ethyl acetate layer is washed
  5. 5
    その他dried
  6. 6
    その他evaporated
  7. 7
    その他to remove the solvent
  8. 8
    その他The residue is crystallized from hexane/ethyl acetate

実験手順

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).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05728706uspto-grants-1998_03