反应详情

温度

67 °C

To 2-chloro-6-(2,4-dichlorophenyl)-5-(4-chlorophenyl)pyridine-3-carbonitrile (2.03 g) in THF (14 mL) was added H2NCH3 (13 mL, 2 M solution in THF). The reaction was heated to 67° C. in a closed vessel for 9 hours before concentrating. The product was dissolved in EtOAc and washed with saturated aqueous NaHCO3 solution. The solution was concentrated and purified via flash chromatography on silica gel with a gradient elution of 0% to 10% EtOAc in hexane affording the title compound. HPLC/MS: 387.8(M+1), 389.8 (M+3); Rt=4.26 min.

1. concentrationbefore concentrating
2. dissolutionThe product was dissolved in EtOAc
3. washwashed with saturated aqueous NaHCO3 solution
4. concentrationThe solution was concentrated
5. custompurified via flash chromatography on silica gel with a gradient elution of 0% to 10% EtOAc in hexane affording the title compound