反应详情

Diethyl 2-phthalimidomalonate (obtained from Aldrich Chemical Company Limited) (9.8 g, 32.0 mmol) and 2-chloro-4-dodecylsulphonylaniline (11.5 g, 32.0 mmol) were added to xylene (250 ml) and refluxed under a Dean and Stark trap for 96 hr. The distillate was periodically removed and the main bulk of solvent replenished as necessary. Removal of the xylene solvent under reduced pressure afforded a light brown oil which was purified by column chromatography using a 4:1 mixture of 60-80° C. petroleum ether:ethyl acetate and silica gel. The product, coupler (C13), was obtained as a white solid which was slurried with a little petroleum ether, filtered and dried in air, 13.6 g, 67%.

1. temperaturerefluxed under a Dean and Stark trap for 96 hr
2. customThe distillate was periodically removed
3. customRemoval of the xylene solvent under reduced pressure
4. customafforded a light brown oil which
5. customwas purified by column chromatography
6. additiona 4:1 mixture of 60-80° C. petroleum ether
7. customThe product, coupler (C13), was obtained as a white solid which
8. filtrationfiltered
9. customdried in air, 13.6 g, 67%