1603-40-3

108-99-6

1603-41-4

1603-40-3

1) Add 9021 g of toluene, 538 g of sodium metal, 70 g of ethanolamine and 1900 g of 3-methylpyridine to the autoclave. After sealing the autoclave, open the feeding ports of the autoclave inlet and drip tank, and make sure the valves of the drip tank and the kettle are open. A hose was extended through the inlet port to the bottom of the kettle, and nitrogen was passed in to displace the air for 1 min, followed by closing the inlet cover. Heat the mixture to 60°C and slowly add liquid ammonia dropwise, maintaining the pressure in the autoclave at 3 MPa, until the total amount of liquid ammonia added reaches 600 g. 2) Increase the reaction temperature to 170°C and fill the autoclave with nitrogen until the pressure reaches 5 MPa to ensure that the reaction is fully carried out. When the pressure in the autoclave rose to 5.5 MPa, the pressure was released to 5 MPa and the process was repeated until the pressure no longer rose due to the reaction, indicating that the reaction was complete. The reaction system was then cooled to room temperature. 3) The ammoniated liquid was slowly added dropwise to 9 kg of water and the mixture was stirred to promote hydrolysis and extraction. After standing, the phases were separated and the aqueous phase was subjected to secondary extraction with 3 L of toluene. All organic phases were combined and the oil phase was quantitatively analyzed by gas chromatography to yield 1928 g of 2-amino-5-methylpyridine and 144 g of 2-amino-3-methylpyridine.