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With sodium carbonate In 1,4-dioxane at 130℃; for 0.5h; microwave irradiation;
2.7
A mixture of tetτakis(triphenylphosphine)palladium(0) (28 mg, 24 μmol), 3-borono-5- fluoro-4-methylbenzoic acid (175 mg, 0.88 mmol) and 5-chloro-l-(2,4-difluorophenyl)-7- ethyl-lH-pyrazolo[4,3-b]pyrazin-6(7H)-one (250 mg, 0.80 mmol) in 4.0 mL dioxane and 2.0 mL of 1 N sodium carbonate was heated in a microwave at 130 0C for 30 min. The reaction mixture was treated with EtOAc (15 mL) and extracted with IN NaOH (3 x 10 mL). The aqueous extracts were treated with 5 N HCl to pH 2 and extracted with DCM (3 x 15 mL). The combined DCM layers were dried over MgSO4, filtered and concentrated affording 3-( 1 -(2,4-difluorophenyl)-7-ethyl-6-oxo-6,7-dihydro- 1 H-pyrazolo[4,3- b]pyrazin-5-yl)-5-fluoro-4-methylbenzoic acid as a light orange-brown viscous oil. This material was used without purification. MS (ES+): 429.1 (M+H)+.
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