反应详情

7-{[2-Chloro-3-(trifluoromethyl)phenyl]carbonyl}-2-(trifluoromethyl)-5,6,7,8-tetrahydroimidazo[1,2-a]pyrazine (0.181 g, 0.455 mmol, Example 2) was dissolved in N,N-dimethylformamide (DMF) (2 mL) and treated with N-bromosuccinimide (NBS, 0.097 g, 0.546 mmol). The solution was stirred at room temperature for 16 hr. The mixture was poured onto water (100 ml) containing 1% sodium sulfite (w/w) and extracted into ethyl acetate (3×50 ml). The combined extracts were washed with brine (50 ml), dried over anhydrous sodium sulfate and concentrated to afford crude product (0.323 g). The crude product was purified by mass-directed automated preparative HPLC to afford 3-bromo-7-{[2-chloro-3-(trifluoromethyl)phenyl]carbonyl}-2-(trifluoromethyl)-5,6,7,8-tetrahydroimidazo[1,2-a]pyrazine (0.135 g, 0.283 mmol, 62.2% yield).

1. additionThe mixture was poured onto water (100 ml)
2. extractionextracted into ethyl acetate (3×50 ml)
3. washThe combined extracts were washed with brine (50 ml)
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationconcentrated
6. customto afford crude product (0.323 g)
7. customThe crude product was purified