反应详情

Ethyl 3-(4-Tributylstannylphenyl)butyrate (5.46 g) and 3-bromo-1-(4-ethylpiperazin-1-yl)isoquinoline (1.33 g) were heated under reflux overnight in the presence of tetrakistriphenylphosphinepalladium(0) (0.19 g) in xylene in nitrogen atmosphere. After cooling, the reaction solution was diluted with ethyl acetate and filtered. The filtrate was extracted with 2N hydrochloric acid. The aqueous layer was washed with ethyl acetate, adjusted to pH 10 with a 8N aqueous solution of sodium hydroxide, and then extracted in ethyl acetate. The organic layer 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 1-(4-ethylpiperazin-1-yl)-3-[4-(1-ethoxycarbonylpropan-2-yl)phenyl]isoquinoline (1.34 g) as a pale yellow viscous oil.

1. temperatureAfter cooling
2. filtrationfiltered
3. extractionThe filtrate was extracted with 2N hydrochloric acid
4. washThe aqueous layer was washed with ethyl acetate
5. extractionextracted in ethyl acetate
6. washThe organic layer 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)