反应详情

A mixture of 1.73 g (0.013 mol) of rhodanine, 2.06 g (0.01 mol) of 3,4-dimethoxybenzalacetone, 0.31 g (0.004 mol) of ammonium acetate and 5 ml of toluene was heated under reflux for 2 hours. After cooling, precipitates were recovered by filtration and washed with methanol. The residue was purified by silica gel column chromatography (eluent, chloroform) to obtain 0.5 g of the isomer A of the desired 5-(α-methyl-3,4-dimethoxycinnamylidene)-4-oxo-2-thioxothiazolidine from the first eluate and 0.2 g of the isomer B from the subsequent eluate.

1. temperaturewas heated
2. temperatureunder reflux for 2 hours
3. temperatureAfter cooling
4. customprecipitates
5. filtrationwere recovered by filtration
6. washwashed with methanol
7. customThe residue was purified by silica gel column chromatography (eluent, chloroform)