Ethanol → 2-(2-Fluoro-5-((4-(methylsulfonyl)piperazin-1-YL)methyl)pyridin-3-YL)-4-methyl-1,3,5-triazine

HRID 1621398Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1621398
[F:1][C:2]1[C:7]([C:8]2[N:13]=[C:12]([CH3:14])[N:11]=[C:10](SC)[N:9]=2)=[CH:6][C:5]([CH2:17][N:18]2[CH2:23][CH2:22][N:21]([S:24]([CH3:27])(=[O:26])=[O:25])[CH2:20][CH2:19]2)=[CH:4][N:3]=1.CCO>[Ni]>[F:1][C:2]1[C:7]([C:8]2[N:13]=[C:12]([CH3:14])[N:11]=[CH:10][N:9]=2)=[CH:6][C:5]([CH2:17][N:18]2[CH2:19][CH2:20][N:21]([S:24]([CH3:27])(=[O:26])=[O:25])[CH2:22][CH2:23]2)=[CH:4][N:3]=1

Komponenten

4

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

Raney nickel (76 mg, 1.297 mmol) water suspension was added to a mixture of 2-(2-fluoro-5-((4-(methylsulfonyl)piperazin-1-yl)methyl)pyridin-3-yl)-4-methyl-6-(methylthio)-1,3,5-triazine (107 mg, 0.259 mmol) in EtOH (5.00 mL, 86 mmol) and the mixture was heated under nitrogen at 70° C. for 1.5 h. The resulting mixture was passed through a short plug of Celite® (diatomaceous earth). The filter cake was washed with MeOH (3×10 mL). The combined organic phases were concentrated to give the crude product, which was used directly in the next step without purification.

Aufarbeitung

  1. washThe filter cake was washed with MeOH (3×10 mL)
  2. concentrationThe combined organic phases were concentrated

Quellen und Nachweise

ORD-Eintrag
ord-bb79c404cb074dcc8614ab2b7e3d5694
Quelldatensatz
uspto-grants-2014_07
Patentnummer
US08772480B2

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