تفاعل #2401

ord-c45d1e41cd734870bba0fc8cf09b8c4c

معادلة التفاعل

[Cl-].[NH4+]
ammonium chloride
Cc1ccc(-c2c(N)ncnc2Cl)cc1
6-chloro-5-(4-methylphenyl)pyrimidin-4-amine
[H-].[Na+]
sodium hydride
OCCO
ethylene glycol
Cc1ccc(-c2c(N)ncnc2OCCO)cc1
2-{6-amino-5-(4-methylphenyl)pyrimidin-4-yloxy}-ethanol

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىis reacted at 70° C. for two hours
  2. 2
    أخرىreacted at 90° C. for five hours
  3. 3
    استخلاصextracted with ethyl acetate
  4. 4
    غسيلThe ethyl acetate layer is washed
  5. 5
    أخرىdried
  6. 6
    أخرىevaporated
  7. 7
    أخرىto remove the solvent
  8. 8
    أخرىThe residue is crystallized from hexane/ethyl acetate

الإجراء التجريبي

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).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05728706uspto-grants-1998_03