反应详情

温度

150 °C

A mixture of 4-chloro-3,6-dimethyl-2-(2,4,6-trimethylphenoxy)-pyridine (1.330 g, 4.822 mmol) and 20 ml of ethyl amine in 13 ml of 1-methyl-2-pyrrolidinone was heated at 150° C. at 250 psi overnight in a pressure reactor. The reaction was heated an additional 24 hours at 175° C. and 300 psi. The reaction mixture cooled to room temperature and diluted with water and extracted with ethyl acetate. The organic layer was dried and concentrated to give a brown oil. The oil residue was purified through silica gel column chromatography using chloroform to 2% methanol in chloroform as eluent to give 0.820 g (60%) of the title compound as a white solid, mp 115–116° C.

1. temperatureThe reaction was heated an additional 24 hours at 175° C.
2. temperatureThe reaction mixture cooled to room temperature
3. extractionextracted with ethyl acetate
4. customThe organic layer was dried
5. concentrationconcentrated
6. customto give a brown oil
7. customThe oil residue was purified through silica gel column chromatography