反应详情

温度

25 °C

To a solution of 3-(3-bromo-5-chlorophenoxy)-4-methylpyridin-2-ol (11-5; 75 mg, 0.238 mmol) and tert-butyl 3-(bromomethyl)-1H-pyrazolo[3,4-b]pyridine-1-carboxylate (74.4 mg, 0.238 mmol) was added potassium carbonate (33 mg, 0.238 mmol) and the resulting mixture was stirred at 25° C. for 18 hours. After this time, the mixture was filtered and then purified on Gilson LC using a Luna column (10μ, C18, 250×21.2 cm) eluting with 5-95% ACN/water with 0.1% TFA). The desired fractions were concentrated to dryness and the resulting solid was dissolved in trifluoroacetic acid (2 mL) This solution was concentrated on the rotary evaporator to give the title compound. LRMS (M+1)=446.7

1. filtrationAfter this time, the mixture was filtered
2. custompurified on Gilson LC
3. washeluting with 5-95% ACN/water with 0.1% TFA)
4. concentrationThe desired fractions were concentrated to dryness
5. dissolutionthe resulting solid was dissolved in trifluoroacetic acid (2 mL) This solution
6. concentrationwas concentrated on the rotary evaporator