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Stage #1: With sodium methylate In methanol at 10 - 35℃; for 0.416667 h; Stage #2: With acetic acid In methanol at 50℃; for 1 h; Stage #3: With hydrogenchloride In methanolReflux
Step 1: 2-(1H-Imidazol-2-yl)pyrazine 2,2-Diethoxyethanamine (3 g, 2.25 mmol) was dissolved in dry methanol (20 mL). To this was added sodium methoxide (1.22 g, 22.5 mmol, as a 25percent solution in methanol). After stirring for 25 minutes at room temperature, pyrazine-2-carbonitrile (2.37 g, 22.5 mmol) and acetic acid (1.35 g, 22.5 mmol) were added and the subsequent solution was stirred at 50° C. for 1 hour. MeOH (40 mL) and 6N HCl (12 mL) were added and the reaction was stirred at reflux overnight. The reaction mixture was cooled to room temperature and partitioned between 1:1 Et2O and water (60 mL) and the layers were separated. The aqueous layer was basified to pH 9/10 and extracted with 10percent MeOH in DCM. The combined organic extracts were dried (MgSO4), filtered and concentrated to give the desired compound (1.49 g yellow solid). 1H NMR (400 MHz, MeOH-d4) δ ppm: 7.67 (s, 1H), 7.09 (d, J=1.8 Hz, 1H), 6.99 (d, J=2.5 Hz, 1H), 5.72 (s, 2H)
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