[CH3:1][O:2][C:3]1[N:8]=[CH:7][N:6]=[C:5]([C:9]#N)[CH:4]=1.[CH:11]1([Mg]Br)[CH2:13][CH2:12]1.Cl.C(=O)([O-])[OH:18].[Na+]>C1COCC1>[CH:11]1([C:9]([C:5]2[CH:4]=[C:3]([O:2][CH3:1])[N:8]=[CH:7][N:6]=2)=[O:18])[CH2:13][CH2:12]1
Under a nitrogen atmosphere, to a solution of 6-methoxypyrimidine-4-carbonitrile (6.00 g) in THF (120 mL) was added dropwise a 0.52 M solution of cyclopropylmagnesium bromide in THF (215 mL) at 0° C., and the mixture was stirred at 0° C. for 1 hr. 6N Hydrochloric acid (60 mL) was added to the reaction mixture at 0° C., and the mixture was stirred at room temperature for 15 min. The reaction mixture was neutralized with sodium hydrogen carbonate (35.0 g), and extracted with ethyl acetate. The extract was washed with water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure to give a crude product of the title compound as a brown oil. This compound was used for the next step without further purification.
Wird geladen…
