反应详情

温度

130 °C

A mixture of tetrakis(triphenylphosphine)palladium(0) (28 mg, 24 μmol), 3-borono-5-fluoro-4-methylbenzoic acid (175 mg, 0.88 mmol) and 5-chloro-1-(2,4-difluorophenyl)-7-ethyl-1H-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° C. for 30 min. The reaction mixture was treated with EtOAc (15 mL) and extracted with 1N NaOH (3×10 mL). The aqueous extracts were treated with 5 N HCl to pH 2 and extracted with DCM (3×15 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-1H-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)+.

1. extractionextracted with 1N NaOH (3×10 mL)
2. additionThe aqueous extracts were treated with 5 N HCl to pH 2
3. extractionextracted with DCM (3×15 mL)
4. dry with materialThe combined DCM layers were dried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated