反应详情

3-Iodo-4-(4-nitrophenoxy)-2-pyridinamine (500 mg), ethyl acrylate (0.3 ml), palladium (II) acetate (30 mg), tributylamine (0.66 ml) and dimethylformaldehyde (5 ml) were stirred at 130° C. for 20 minutes. After returning the reaction solution to room temperature, water was added and extraction was performed with ethyl acetate. NH type silica gel was added to the extract, the solvent was distilled off under reduced pressure, and there action product was adsorbed onto the silica gel. The silica gel was charged into a dry column packed with NH type silica gel, and column purification was performed (hexane:ethyl acetate=3:1). The solvent was distilled off under reduced pressure to obtain 330 mg of the target substance as a yellow oil.

1. customto room temperature
2. extractionextraction
3. additionNH type silica gel was added to the extract
4. distillationthe solvent was distilled off under reduced pressure, and there action product
5. additionThe silica gel was charged into a dry column
6. custompacked with NH type silica gel, and column purification
7. distillationThe solvent was distilled off under reduced pressure
8. customto obtain 330 mg of the target substance as a yellow oil