反应详情

温度

90 °C

To a degassed solution of the product of Example 5 (70 mg, 0.23 mmol) in N,N-dimethylacetamide (2 ml) was added 2-tributylstannylbenzonitrile (183 mg, 0.46 mmol), lithium chloride (27.5 mg, 0.58 mmol), copper(I) iodide (5 mg) and dichloro[1,1′-bis(diphenylphosphino)ferrocene]palladium(II) (9 mg) and the mixture heated at 90° C. for 4 h. After cooling to ambient temperature the reaction was poured onto a strong cation exchange cartridge and eluted with methanol. The product was then eluted with a 2.0M solution of ammonia in methanol and evaporated in vacuo. The residue was dissolved in 5% methanol in dichloromethane and applied to two preparative TLC plates (silica gel) and eluted with 1:1 ethyl acetate in isohexane. The appropriate band was collected and processed to give a solid which was recrystallised from dichloromethane/ethyl acetate/isohexane to give 2-[4-(7-trifluoromethylimidazo[1,2-α]pyrimidin-3-yl)pyrimidin-2-yl]benzonitrile (10 mg) as a white solid: δH (400 MHz, CDCl3) 7.50 (1H, d, J 7.4), 7.65-7.69 (1H, m), 7.78-7.82 (2H, m), 7.94 (1H, dd, J 7.8 and 1.2), 8.34 (1H, dd, J 8.0 and 1.0), 8.74 (1H, s), 8.97 (1H, d, J 5.5), 10.74 (1H, d, J 7.4); m/z (ES+) 366 (M++H).

1. temperatureAfter cooling to ambient temperature the reaction
2. additionwas poured onto a strong cation exchange cartridge
3. washeluted with methanol
4. washThe product was then eluted with a 2.0M solution of ammonia in methanol
5. customevaporated in vacuo
6. dissolutionThe residue was dissolved in 5% methanol in dichloromethane
7. washeluted with 1:1 ethyl acetate in isohexane
8. customThe appropriate band was collected
9. customto give a solid which
10. customwas recrystallised from dichloromethane/ethyl acetate/isohexane