反应详情

温度

95 °C

To a mixture of 6-bromo-3-[((2S)-2-methyl-4-{[4-(trifluoromethyl)phenyl]sulfonyl}-1-piperazinyl)carbonyl]pyrazolo[1,5-a]pyrimidine (may be prepared as described in Example 12) (300 mg, 0.564 mmol) and 1,1′-bis(diphenylphosphino)ferrocene (39.1 mg, 0.070 mmol) under argon in dry N,N-dimethylformamide (6 mL) was added zinc cyanide (86 mg, 0.733 mmol) followed by tris(dibenzylideneacetone)dipalladium(0) (32.0 mg, 0.035 mmol) and the mixture heated to 95° C. for 2 h. The mixture was partitioned between ethyl acetate (30 mL) and aqueous sodium bicarbonate (20 mL). The organic phase was washed with further sodium bicarbonate (10 mL), water (10 mL) and brine (10 mL) before it was dried (MgSO4), filtered and the solvent removed in vacuo. Half the crude material was purified by MDAP and the solvent evaporated to give the title compound (67 mg) as a yellow solid.

1. customThe mixture was partitioned between ethyl acetate (30 mL) and aqueous sodium bicarbonate (20 mL)
2. washThe organic phase was washed with further sodium bicarbonate (10 mL), water (10 mL) and brine (10 mL) before it
3. dry with materialwas dried (MgSO4)
4. filtrationfiltered
5. customthe solvent removed in vacuo
6. customHalf the crude material was purified by MDAP
7. customthe solvent evaporated