反应详情

A mixture of 20.2 g of 19A and 14.8 g of phthalic anhydride in 300 mL of toluene was treated with 1.01 g of triethylamine and heated to reflux for 16 hours with a Dean-stark trap to effect azeotropic removal of water. The toluene was removed in vacuo, the residue was dissolved in 800 mL of methylene chloride, and treated with 35 g charcoal. After filtration through celite and concentration of solvent in vacuo, the residue was recrystallized from ethanol to afford N-[3-(allyloxy)-4-chloro-6-fluorophenyl]phthalimide (41A) as tan crystals, m.p.: 148°-150° C.

1. temperatureheated
2. temperatureto reflux for 16 hours with a Dean-stark trap
3. customremoval of water
4. customThe toluene was removed in vacuo
5. dissolutionthe residue was dissolved in 800 mL of methylene chloride
6. additiontreated with 35 g charcoal
7. filtrationAfter filtration through celite and concentration of solvent in vacuo
8. customthe residue was recrystallized from ethanol