反应详情

温度

145 °C

2-Morpholinoethanol (2.21 g, 16.8 mmol) was treated with sodium (0.407 g, 17.7 mmol) until a homogeneous suspension was obtained. 4-Chloropyridin-2-amine (1.14 g, 8.86 mmol) was added and the mixture was heated with magnetic stirring at 145° C. in a sealed tube for 10 hours. The reaction mixture was cooled and diluted with water and EtOAc. The layers were separated, and the aqueous phase was extracted twice with EtOAc. The combined organic extracts were concentrated to afford a viscous oil which was subjected to chromatographic purification on silica with 10% MeOH/DCM as eluent to provide 1.37 g of desired product as a low-melting solid.

1. customwas obtained
2. temperaturethe mixture was heated
3. temperatureThe reaction mixture was cooled
4. customThe layers were separated
5. extractionthe aqueous phase was extracted twice with EtOAc
6. concentrationThe combined organic extracts were concentrated
7. customto afford a viscous oil which
8. customwas subjected to chromatographic purification on silica with 10% MeOH/DCM as eluent