反应详情

A mixture of 12.28 g of 2-butyl-6-iodo-4(1H)-quinazolinone 0.866 g of tetrakis (triphenylphosphine)palladium, 0.015 g of 2,6-di-t- butyl-4-methylphenol in 75 ml of toluene and 20 ml of N,N-dimethylformamide is treated with 13.06 g of tri-n-butyl vinyltin followed by heating at reflux for 4 hours. The reaction mixture is cooled and concentrated in vacuo. The residue is diluted with hexanes and filtered. The filter cake is washed with hexanes and the remaining tacky solid dissolved in 100 ml of chloroform-reethanol (8:2) and purified by chromatography on silica gel with 1:3 ethyl acetate-hexanes to afford 4.55 g of the desired product as a yellow solid. CI MASS SPEC 229MH+).

1. temperatureby heating
2. temperatureat reflux for 4 hours
3. temperatureThe reaction mixture is cooled
4. concentrationconcentrated in vacuo
5. additionThe residue is diluted with hexanes
6. filtrationfiltered
7. washThe filter cake is washed with hexanes
8. dissolutionthe remaining tacky solid dissolved in 100 ml of chloroform-reethanol (8:2)
9. custompurified by chromatography on silica gel with 1:3 ethyl acetate-hexanes