反应详情

温度

50 °C

To a solution of 1-(3-chloro-4-methoxyphenyl)-N-(6′-methoxy-3,5′-dimethyl-2,3′-bipyridin-6-yl)cyclopropanecarboxamide (44 mg, 0.10 mmol) in acetonitrile (2 mL) was added TMS-Iodide (57.2 μL, 0.40 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 (10-99% CH3CN in water). ESI-MS m/z calc. 423.1. found 424.3 (M+1)+. Retention time 1.52 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 (10-99% CH3CN in water)