反应详情

温度

120 °C

A mixture of N′-[3-(3-bromo-5-chlorophenoxy)-4-methylpyridin-2-yl]-2-(1H-pyrazolo[3,4-b]pyridin-3-yl)acetohydrazide (44 mg, 0.090 mmol) in phosphorus oxychloride (250 μL, 2.6 mmol) was heated to 120° C. for 35 minutes, after which the excess reagent was removed in vacuo and the residue partitioned between saturated aqueous NaHCO3 (20 mL) and CH2Cl2 (2×20 mL). The combined extracts were concentrated in vacuo and the residue was purified on a Luna column (10μ, C18, 250×21.2 cm) eluting with 5-95% ACN/water with 0.1% TFA) to give the title compound. LRMS (M+1)=470.7.

1. customafter which the excess reagent was removed in vacuo
2. customthe residue partitioned between saturated aqueous NaHCO3 (20 mL) and CH2Cl2 (2×20 mL)
3. concentrationThe combined extracts were concentrated in vacuo
4. customthe residue was purified on a Luna column (10μ, C18, 250×21.2 cm)
5. washeluting with 5-95% ACN/water with 0.1% TFA)