反应详情

温度

50 °C

To a solution of N-(6′-methoxy-3,5′-dimethyl-2,3′-bipyridin-6-yl)-1-(3-methoxyphenyl)cyclopropanecarboxamide (41 mg, 0.10 mmol) in acetonitrile (2 mL) was added TMS-Iodide (28.0 μL, 0.20 mmol). The reaction was stirred at 50° C. for 20 min. The reaction solution was diluted with dichloromethane and washed with saturated NaHSO3 (2×), brine, dried over MgSO4 and concentrated. The crude product was dissolved in DMSO (1 mL) and purified by reverse phase HPLC (Gilson, 10-99% CH3CN in water) to yield the desired product. ESI-MS m/z calc. 389.4. found 390.5 (M+1)+. Retention time 1.41 minutes.

1. washwashed with saturated NaHSO3 (2×), brine
2. dry with materialdried over MgSO4
3. concentrationconcentrated
4. dissolutionThe crude product was dissolved in DMSO (1 mL)
5. custompurified by reverse phase HPLC (Gilson, 10-99% CH3CN in water)