反应详情

2-Methoxy-5-tributylstannylpyridine (1.41 g) and 3-bromo-1-(4-ethylpiperazin-1-yl)isoquinoline (0.57 g) obtained in Example 28-2 were heated under reflux in the presence of tetrakistriphenylphosphinepalladium(0) (0.10 g) in xylene in nitrogen atmosphere for 30 min. After cooling, the reaction solution was filtered and extracted in 2N hydrochloric acid. The aqueous layer was washed with ethyl acetate twice. The resulting aqueous layer was adjusted to pH 10 with a 8N aqueous solution of sodium hydroxide, and then extracted with ethyl acetate. The extract was washed with a 10% aqueous solution of sodium carbonate and brine, and dried over magnesium sulfate. The solvent was evaporated, and the resulting residue was purified by silica gel column chromatography (chloroform/methanol system), to give 0.38 g of the free compound of the title compound as a pale brown powder.

1. temperatureAfter cooling
2. filtrationthe reaction solution was filtered
3. extractionextracted in 2N hydrochloric acid
4. washThe aqueous layer was washed with ethyl acetate twice
5. extractionextracted with ethyl acetate
6. washThe extract was washed with a 10% aqueous solution of sodium carbonate and brine
7. dry with materialdried over magnesium sulfate
8. customThe solvent was evaporated
9. customthe resulting residue was purified by silica gel column chromatography (chloroform/methanol system)