反应详情

To a stirred suspension of 5-methyl-2-nitroaniline (10.0 g) in ethanol (20 ml) were added 2,2-dimethyl-1,3-dioxane-4,6-dione (9.95 g) and triethyl orthoformate (10.7 g) at 50° C. The resulting mixture was heated at 120° C. for one hour during which time ethanol (20 ml) was added to the mixture and ethanol liberated was distilled off. After cooling, ethyl acetate (40 ml) was added thereto and the resulting precipitate was collected by filtration. The solid was washed with hot ethanol (40 ml) and allowed to cool to ambient temperature. The precipitate was collected by filtration and air-dried to afford isopropylidene (5-methyl-2-nitroanilino)methylenemalonate (15.2 g) as yellow needles.

1. distillationliberated was distilled off
2. temperatureAfter cooling
3. additionethyl acetate (40 ml) was added
4. filtrationthe resulting precipitate was collected by filtration
5. washThe solid was washed with hot ethanol (40 ml)
6. filtrationThe precipitate was collected by filtration
7. customair-dried