[CH3:1][Mg]Br.[C:4]([C:6]1[C:11]([F:12])=[CH:10][C:9]([F:13])=[CH:8]N=1)#N.OS(O)(=O)=O.[NH4+:19].[OH-:20]>C(OCC)C.C1COCC1>[F:12][C:11]1[C:6]([C:4](=[O:20])[CH3:1])=[N:19][CH:8]=[C:9]([F:13])[CH:10]=1Methylmagnesium bromide (10 ml of a 3N solution in diethylether) were added drop-wise with stirring to a solution of 15 g (10.71 mmol) 2-cyano-3,5-difluoropyridine in 100 ml THF at 0° C. and the mixture was subsequently stirred at room temperature until reaction was complete. For workup the mixture was acidified with 10% H2SO4 to pH 4, was subsequently made basic with 25% NH4OH, was extracted 2× with dichloromethane, and the combined organic phases were dried with MgSO4. Purification by chromatography on silica gel (dichloromethane/methanol 0-5%) yielded 500 mg of a light colored oil, which crystallized upon being left to stand.
Wird geladen…
