反应详情

温度

100 °C

2-bromo-5-iodopyrazine (503 mg, 1.77 mmol) and tert-butyl piperazine-1-carboxylate (355 mg, 1.91 mmol) were taken up in tBuOH (8 mL). iPr2NEt (400 μL, 2.3 mmol) was added and the stirred reaction mixture was heated to 100° C. After 66 h, the reaction mixture was cooled and was partitioned between EtOAc, water and brine. The phases were separated, and the organic phase was dried over Na2SO4, filtered, and concentrated. The crude residue was purified by silica gel chromatography (10-30% EtOAc in hexanes) to afford tert-butyl 4-(5-iodopyrazin-2-yl)piperazine-1-carboxylate 7.11.

1. customthe stirred reaction mixture
2. temperaturethe reaction mixture was cooled
3. customwas partitioned between EtOAc, water and brine
4. customThe phases were separated
5. dry with materialthe organic phase was dried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated
8. customThe crude residue was purified by silica gel chromatography (10-30% EtOAc in hexanes)