反应详情

温度

0 °C

To 5-(5-aminopyrazin-2-yl)piperidin-2-one (25 mg, 0.13 mmol) acetonitrile (10 mL) solution at 0° C. was added NBS (23.2 mg, 0.13 mmol) and the reaction mixture was stirred at 0° C. for 30 min, then at room temperature for 4 h. The reaction mixture was concentrated, and the residue was basified by 1 N NaOH (140 ul), diluted with methanol (2 mL), concentrated. The residue was triturated with EtOAc (3×1 mL), and the EtOAc supernatants were collected, combined and concentrated and a light solid was obtained as crude 5-(5-amino-6-bromopyrazin-2-yl)piperidin-2-one which was used in next step without further purification. LCMS (m/z): 241/243 (MH+), 0.41 min.

1. waitat room temperature for 4 h
2. concentrationThe reaction mixture was concentrated
3. additiondiluted with methanol (2 mL)
4. concentrationconcentrated
5. customThe residue was triturated with EtOAc (3×1 mL)
6. customthe EtOAc supernatants were collected
7. concentrationconcentrated