Reaktion #9996

ord-3a5c495ce8bd459ab04cfd5ab755e0c5

Reaktionsgleichung

CCn1cnc2c(Nc3cccc(C(F)(F)F)c3)nc(Cl)nc21
2-chloro-9-ethyl-6-(3-trifluoromethyl-phenyl-amino)-9H-purine
NCCCO
3-amino-1-propanol
CCn1cnc2c(Nc3cccc(C(F)(F)F)c3)nc(NCCCO)nc21
9-Ethyl-2-(3-hydroxy-propyl-amino)-6-(3-trifluoromethyl-phenyl-amino)-9H-purine

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturto cool
  2. 2
    WaschenThe organic phase is washed with water
  3. 3
    Trocknendried over sodium sulfate
  4. 4
    SonstigeAfter removal of the solvent
  5. 5
    Sonstigethe residue is recrystallized from ethyl acetate and diethyl ether

Vorschrift

200 mg (0.58 mmol) of 2-chloro-9-ethyl-6-(3-trifluoromethyl-phenyl-amino)-9H-purine and 2 ml of 3-amino-1-propanol are stirred at 140° C. for 2 h and the mixture is allowed to cool and is diluted with 60 ml of ethyl acetate. The organic phase is washed with water and dried over sodium sulfate. After removal of the solvent, the residue is recrystallized from ethyl acetate and diethyl ether. 9-Ethyl-2-(3-hydroxy-propyl-amino)-6-(3-trifluoromethyl-phenyl-amino)-9H-purine is obtained; m.p. 136–137° C.; FAB-MS: (M+H)+=381; Rf=0.7 (ethyl acetate:methanol=9:1).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07091346B1uspto-grants-2006_08