反应详情

To a mixture of 0.66 g (1.2 mmol) of tert-butyl 4-[2-(4-fluorophenyl)-3-iodo-7,8-dimethylimidazo[1,2-b]pyridazin-6-yl]piperazine-1-carboxylate in 15 mL of a mixture of tetrahydrofuran and water (9:1), are added 1.17 g (3.6 mmol) of cesium carbonate and 0.31 g (1.4 mmol) of (pyrid-4-yl)boronic acid. After sparging with a stream of argon for a few moments, 88 mg (0.11 mmol) of a complex of [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) and dichloromethane (PdCl2(dppf).CH2Cl2) are added and the reaction mixture is refluxed under argon for 18 hours. The mixture is then poured into water and the product is extracted with dichloromethane, the organic phase is dried over sodium sulfate and filtered, and the solvent is evaporated off to give a brown solid. The product is purified by chromatography on silica gel, eluting with a mixture of ethyl acetate and cyclohexane (3/7) to give 0.44 g of a white powder.

1. additionare added
2. temperaturethe reaction mixture is refluxed under argon for 18 hours
3. extractionthe product is extracted with dichloromethane
4. dry with materialthe organic phase is dried over sodium sulfate
5. filtrationfiltered
6. customthe solvent is evaporated off
7. customto give a brown solid
8. customThe product is purified by chromatography on silica gel
9. washeluting with a mixture of ethyl acetate and cyclohexane (3/7)