3-Amino-1-propanol → 9-Ethyl-2-(3-hydroxy-propyl-amino)-6-(3-trifluoromethyl-phenyl-amino)-9H-purine

HRID 9900

Reaktionsgleichung

Reaktionsgleichung von HRID 9900
Cl[C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][N:8]2[CH2:11][CH3:12])=[C:4]([NH:13][C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([C:20]([F:23])([F:22])[F:21])[CH:15]=2)[N:3]=1.[NH2:24][CH2:25][CH2:26][CH2:27][OH:28]>C(OCC)(=O)C>[CH2:11]([N:8]1[CH:7]=[N:6][C:5]2[C:9]1=[N:10][C:2]([NH:24][CH2:25][CH2:26][CH2:27][OH:28])=[N:3][C:4]=2[NH:13][C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([C:20]([F:23])([F:22])[F:21])[CH:15]=1)[CH3:12]

Komponenten

4

Edukt 2

HCID 90863-Amino-1-propanolHCID 219881872-chloro-9-ethyl-6-(3-trifluoromethyl-phenyl-amino)-9H-purine

Produkt 1

HCID 219882069-Ethyl-2-(3-hydroxy-propyl-amino)-6-(3-trifluoromethyl-phenyl-amino)-9H-purine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

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).

Aufarbeitung

  1. temperatureto cool
  2. washThe organic phase is washed with water
  3. dry with materialdried over sodium sulfate
  4. customAfter removal of the solvent
  5. customthe residue is recrystallized from ethyl acetate and diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-3a5c495ce8bd459ab04cfd5ab755e0c5
Quelldatensatz
uspto-grants-2006_08
Patentnummer
US07091346B1

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