反应详情

温度

120 °C

140 mg (0.50 mmol) of N-[4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridin-2-yl]cyclopropanecarboxamide and 172 mg (1.2 eq 0.60 mmol) of 3-bromo-2-(4-fluorophenyl)-5,6-dihydro-4H-pyrrolo[1,2-b]pyrazole are dissolved in 3.5 mL 1,4-dioxan. To this are added 36 mg of bis(tricyclohexylphosphine)-palladium(II)dichloride (0.05 mmol, 0.1 eq) and 1.2 mL sodium carbonate solution (2M in H2O). The reaction mixture is flushed for 5 mins with argon and then sealed. Next the mixture is heated for 12 mins at 120° C. in the microwave (CEM Explorer). After cooling, insoluble components are filtered off and the salt residue washed with 1,4-dioxan. The organic phase is evaporated and the crude product purified by silica gel chromatography (eluent cyclohexane/ethyl acetate). 85 mg (43%) of N-{4-[2-(4-fluorophenyl)-5,6-dihydro-4H-pyrrolo[1,2-b]pyrazol-3-yl]pyridin-2-yl}cyclopropanecarboxamide are obtained as a colourless solid.

1. customThe reaction mixture is flushed for 5 mins with argon
2. customsealed
3. temperatureAfter cooling
4. filtrationinsoluble components are filtered off
5. washthe salt residue washed with 1,4-dioxan
6. customThe organic phase is evaporated
7. customthe crude product purified by silica gel chromatography (eluent cyclohexane/ethyl acetate)