2-Methoxyethanol → 6-Chloro-4-(2-methoxyethoxy)pyrido[3,2-d]pyrimidin-2-amine

HRID 1517459Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1517459
CC(C)([O-])C.[K+].[Cl:7][C:8]1[CH:9]=[CH:10][C:11]2[N:12]=[C:13]([NH2:23])[N:14]=[C:15](N3C=NC=N3)[C:16]=2[N:17]=1.[CH3:24][O:25][CH2:26][CH2:27][OH:28]>C(Cl)Cl>[Cl:7][C:8]1[CH:9]=[CH:10][C:11]2[N:12]=[C:13]([NH2:23])[N:14]=[C:15]([O:28][CH2:27][CH2:26][O:25][CH3:24])[C:16]=2[N:17]=1

Komponenten

5

Edukt 3

HCID 80192-MethoxyethanolHCID 23665647Potassium tert-butoxideHCID 576983146-Chloro-4-(1H-1,2,4-triazol-1-yl)pyrido[3,2-d]pyrimidin-2-amine

Produkt 1

HCID 576983626-Chloro-4-(2-methoxyethoxy)pyrido[3,2-d]pyrimidin-2-amineAusbeute 90 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

Potassium t-butoxide (4 mL, 4 mmol; 1 M in THF) was added to a suspension mixture of 6-chloro-4-[1,2,4]triazol-1-yl-pyrido[3,2-d]pyrimidin-2-ylamine (1 g, 4 mmol) and 2-methoxyethanol (0.32 mL, 4 mmol) in DCM (50 mL). After stirring at room temperature for 10 minutes, the mixture was diluted with DCM (100 mL) and washed with brine. The organic layer was dried over Na2SO4 and concentrated to afford the pure title compound as a beige solid (0.91 g, yield 90%) which was characterised as follows: MS (m/z) 225.0 [M+H]+.

Aufarbeitung

  1. washwashed with brine
  2. dry with materialThe organic layer was dried over Na2SO4
  3. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-68428d243fe846e992ebb25473db4967
Quelldatensatz
uspto-grants-2012_07
Patentnummer
US08232278B2

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