反应详情

温度

88 °C

A stirred mixture of 6-bromo-2-[2-(3,5-dimethoxyphenyl)ethyl]-5-(phenylsulfonyl)-5H-pyrrolo[2,3-b]pyrazine (from example 1, step 4, 20.0 mg, 0.0398 mmol), [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) complexed with dichloromethane (1:1) (1.30 mg, 1.59 μmol), N,N-dimethyl-2-[4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazol-1-yl]ethanamine (8.44 mg, 0.0318 mmol), and potassium phosphate (13.5 mg, 0.0637 mmol) in water (0.2 mL)/1,4-dioxane (0.4 mL) was heated at 88° C. After 1 hour, the volatiles were removed under vacuum and the residues were dissolved in methanol (2.0 mL). Potassium carbonate (8.8 mg, 63.7 μmol) was added and the reaction mixture was warmed up to 60° C. After 1 hour, the reaction mixture was cooled to ambient temperature and was purified on RP-HPLC (XBridge C18 column, eluting with a gradient of acetonitrile/water containing 0.05% TFA, at flow rate of 30 mL/min) to give the desired product (3.0 mg) as its TFA salt. LCMS calculated for C23H29N6O2 (M+H)+: m/z=421.2. Found: 421.2.

1. customthe volatiles were removed under vacuum
2. dissolutionthe residues were dissolved in methanol (2.0 mL)
3. temperaturethe reaction mixture was warmed up to 60° C
4. waitAfter 1 hour
5. temperaturethe reaction mixture was cooled to ambient temperature
6. customwas purified on RP-HPLC (XBridge C18 column
7. washeluting with a gradient of acetonitrile/water containing 0.05% TFA, at flow rate of 30 mL/min)