反应详情

Add methyl 2,6-dichloroisonicotinate (3.0 g, 15.0 mmol), trans-dichlorobis(tri-o-tolylphosphine)palladium (II) (196 mg, 0.25 mmol), tributyltin methoxide (2.4 g, 7.5 mmol) and toluene (20 mL) in a previously nitrogen filled sealed vessel. Flush the reactants with nitrogen again. Add isopropenyl acetate (0.85 mL, 7.75 mmol) under nitrogen and heat the sealed mixture at 100° C. overnight with vigorous stirring. Cool the reaction to room temperature, dilute with diethyl ether and filter through a filtering agent. Concentrate and purify (silica gel chromatography, eluting with 0:100 to 20:80 ethyl acetate:hexanes) to give the title compound (29%).

1. additionfilled
2. customsealed vessel
3. customFlush the reactants with nitrogen again
4. temperatureCool
5. customthe reaction to room temperature
6. filtrationfilter through a filtering agent
7. concentrationConcentrate
8. custompurify
9. wash(silica gel chromatography, eluting with 0:100 to 20:80 ethyl acetate:hexanes)