反应详情

A mixture of N-{5-bromo-6-[2-(5-methylthiopyrimidin-2-yloxy)ethoxy]-pyrimidin-4-yl}-4-tert-butylbenzenesulfonamide (200 mg), 2-benzothienyl tributyltin (460 mg), bis(triphenylphosphine)palladium (II) chloride (51 mg), triphenylphosphine (28 mg), copper (I) bromide (21 mg), a few crystals of 2,6-di-tert-butylcresol and dioxane (6 ml) is refluxed for two hours. After cooling, the reaction solution is diluted with ethyl acetate and an aqueous potassium fluoride solution, and the mixture is stirred at room temperature for 60 minutes. The insoluble materials are removed by filtration, and the filtrate is extracted with ethyl acetate. The ethyl acetate layer is washed, dried, and evaporated under reduced pressure to remove the solvent. The residue is purified by silica gel column chromatography (solvent; methylene chloride:acetone=30:1), and recrystallized from ethyl acetate to give the title compound (182 mg).

1. temperatureAfter cooling
2. customThe insoluble materials are removed by filtration
3. extractionthe filtrate is extracted with ethyl acetate
4. washThe ethyl acetate layer is washed
5. customdried
6. customevaporated under reduced pressure
7. customto remove the solvent
8. customThe residue is purified by silica gel column chromatography (solvent; methylene chloride:acetone=30:1)
9. customrecrystallized from ethyl acetate