反应详情

温度

70 °C

To a 50-mL round-bottomed flask was added 3-((6-methoxy-2-pyridinyl)methyl)-2,5-piperazinedione (423 mg, 1.80 mmol), borane methyl sulfide, complex (0.68 mL, 7.19 mmol, Aldrich, St. Louis, Mo.), and THF (6 mL). The reaction mixture was stirred at 70° C. for 2 h and allowed to cool to room temperature. The reaction mixture was diluted with MeOH (1 mL), followed by 1N NaOH (12 mL), and extracted with DCM (2×50 mL). The organic extracts were washed with saturated NaCl (10 mL) and dried over Na2SO4. The solution was filtered and concentrated in vacuo to give the crude 2-((6-methoxy-2-pyridinyl)methyl)piperazine as light-yellow viscous oil, which was used without purification.

1. temperatureto cool to room temperature
2. extractionextracted with DCM (2×50 mL)
3. washThe organic extracts were washed with saturated NaCl (10 mL)
4. dry with materialdried over Na2SO4
5. filtrationThe solution was filtered
6. concentrationconcentrated in vacuo