CON(C)[C:4]([C:6]1[CH:11]=[CH:10][N:9]=[N:8][CH:7]=1)=[O:5].[CH3:13][Mg]Br.[Cl-].[Na+]>O1CCCC1>[N:9]1[CH:10]=[CH:11][C:6]([C:4](=[O:5])[CH3:13])=[CH:7][N:8]=1To N-methoxy-N-methylpyridazine-4-carboxamide (1.13 g, 6.76 mmol) in tetrahydrofuran (22 mL), methylmagnesium bromide (10.1 mL, 10.1 mmol, 1M in diethyl ether) was added dropwise at 0° C. in a nitrogen stream, and the resulting solution was stirred for 1 hour. After completion of the reaction, the reaction solution was mixed with saturated aqueous sodium chloride and extracted with chloroform, and the extract was dried over anhydrous sodium sulfate and evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography (hexane/ethyl acetate=1/2→0/1) to give the desired product (42% yield).
Wird geladen…