反应详情

温度

50 °C

To a solution of 1-(1,3-dihydroisobenzofuran-5-yl)-N-(6′-methoxy-3,5′-dimethyl-2,3′-bipyridin-6-yl)cyclopropanecarboxamide (40 mg, 0.1 mmol) in acetonitrile (2 mL) was added TMS-Iodide (54.8 μL, 0.39 mmol). The reaction was stirred at 50° C. for 20 min. The reaction solution was diluted with CH2Cl2 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/water). ESI-MS m/z calc. 401.1. found 402.5 (M+1)+. Retention time 1.29 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/water)