Potassium Carbonate → HCID 86725664, Verbindung

HRID 878714

Reaktionsgleichung

CS(O[CH2:6][CH2:7][C:8]1[CH:9]=[N:10][N:11]([C:13]2[CH:18]=[C:17]([C:19]#[N:20])[CH:16]=[CH:15][N:14]=2)[CH:12]=1)(=O)=O.[F:21][C:22]1[CH:30]=[CH:29][C:25]([CH2:26][NH:27][CH3:28])=[CH:24][CH:23]=1.C([O-])([O-])=O.[K+].[K+]>C(#N)C>[F:21][C:22]1[CH:30]=[CH:29][C:25]([CH2:26][N:27]([CH3:28])[CH2:6][CH2:7][C:8]2[CH:9]=[N:10][N:11]([C:13]3[CH:18]=[C:17]([C:19]#[N:20])[CH:16]=[CH:15][N:14]=3)[CH:12]=2)=[CH:24][CH:23]=1

Komponenten

Reaktionsbedingungen

Temperatur: 80 °C

Versuchsvorschrift

To a mixture of 2-[1-(4-cyanopyridin-2-yl)pyrazol-4-yl]ethyl methanesulfonate (476 mg, 1.6 mmol) and (4-fluoro-benzyl)-methyl-amine (444 mg, 3.2 mmol) in ACN (30 mL) at rt was added K2CO3 (4.5 g, 32 mmol) and KI (1.0 g, 6.2 mmol. The reaction mixture was heated to 80° C. and stirred overnight. Filtered, solvent removed and purified by prep-HPLC to give the title compound (270 mg, 50%). [M+H] Calc'd for C19H18FN5, 336; Found, 336.

Aufarbeitung

filtrationFiltered
customsolvent removed
custompurified by prep-HPLC

Quellen und Nachweise

ORD-Eintrag: ord-89e19dcb208b474e9683f7b400a39001
Quelldatensatz: uspto-grants-2015_03
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US08987461B2

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