3-(Trifluoromethyl)aniline → 2-Chloro-6-(3-trifluoromethyl-phenyl-amino)-purine

HRID 9901

Reaktionsgleichung

Reaktionsgleichung von HRID 9901
[Cl:1][C:2]1[N:10]=[C:9]2[C:5]([NH:6][CH:7]=[N:8]2)=[C:4](Cl)[N:3]=1.[F:12][C:13]([F:22])([F:21])[C:14]1[CH:15]=[C:16]([CH:18]=[CH:19][CH:20]=1)[NH2:17].C(OCC)(=O)C>C(O)CCC.CN(C=O)C>[Cl:1][C:2]1[N:10]=[C:9]2[C:5]([NH:6][CH:7]=[N:8]2)=[C:4]([NH:17][C:16]2[CH:18]=[CH:19][CH:20]=[C:14]([C:13]([F:12])([F:21])[F:22])[CH:15]=2)[N:3]=1

Komponenten

6

Edukt 3

HCID 73753-(Trifluoromethyl)anilineHCID 8857Ethyl AcetateHCID 53244122,6-Dichloropurine

Produkt 1

HCID 219882372-Chloro-6-(3-trifluoromethyl-phenyl-amino)-purine

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 2631-ButanolLösungsmittelHCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
40 °C

Versuchsvorschrift

1.9 g (10 mmol) of 2,6-dichloro-purine and 8.05 g (50 mmol) of 3-trifluoromethyl-aniline (Fluka, Buchs, Switzerland) in 60 ml of n-butanol and 3 ml of DMF are stirred at 60° C. for 6 h. 50 ml of ethyl acetate are added to the cooled reaction solution and the precipitate is filtered off and further stirred in 40 ml of isopropanol at 40° C. for 60 min. After filtration with suction and drying, 2-chloro-6-(3-trifluoromethyl-phenyl-amino)-purine is obtained; m.p. 248–250° C.; FAB-MS: (M+H)+=314; Rf=0.45 (methylene chloride:methanol=95:5).

Aufarbeitung

  1. filtrationthe precipitate is filtered off
  2. filtrationAfter filtration with suction
  3. customdrying

Quellen und Nachweise

ORD-Eintrag
ord-2af4c11d8f47436cb6ca27b9d322a6e7
Quelldatensatz
uspto-grants-2006_08
Patentnummer
US07091346B1

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