反应详情

温度

100 °C

To a solution of 4-[1-(1-methyl-2-{4-[(1-methyl-1H-pyrazol-3-yl)sulfonyl]piperazin-1-yl}ethyl)-1H-pyrazol-4-yl]-7-{[2-(trimethylsilyl)ethoxy]methyl}-7H-pyrrolo[2,3-d]pyrimidine (0.243 g, 0.415 mmol) in acetonitrile (10 mL) and water (1 mL; ˜8% water/acetonitrile) was added lithium tetrafluoroborate (1.02 g, 10.7 mmol). The solution was refluxed at 100° C. overnight. The mixture was cooled down and 7.2 M of ammonium hydroxide in water (0.346 mL, 2.49 mmol) was added in portions over a period of 5 min at RT, adjusting pH to 9-10 with stirring for 2 h. The solids were removed by filtration and the filtrate was purified on RP-HPLC (XBridge C-18 Column, eluting with a gradient of acetonitrile/water containing 0.15% NH4OH, at flow rate 60 mL/min) to give the desired product (0.159 g, 84.1%). LCMS calculated for C20H26N9O2S(M+H)+: m/z=456.2; Found: 456.4.

1. temperatureThe mixture was cooled down
2. customThe solids were removed by filtration
3. customthe filtrate was purified on RP-HPLC (XBridge C-18 Column
4. washeluting with a gradient of acetonitrile/water containing 0.15% NH4OH, at flow rate 60 mL/min)