反应详情

温度

80 °C

16 gm of 2-[o-(β-chloro-ethoxy)-styryl]-pyridine (m.p. 57°-59° C.) were dissolved in 50 ml of methanol, the solution was mixed at -15° C. with 120 ml of liquid methylamine freshly removed from a bomb, and the mixture was heated at 80° C. in an autoclave for 4 hours. After cooling and releasing the pressure, the contents of the autoclave were evaporated, the residue was dissolved in dilute acetic acid, and the solution was extracted twice with ether to remove weakly basic products. Then, the aqueous phase was made alkaline with 2 N sodium hydroxide solution and was extracted with ethyl acetate. After drying the ethyl acetate extract with sodium sulfate and distilling off the solvent, an oily residue was obtained which crystallized after standing overnight. 13.6 gm (88.2% of theory) of 2-[o-(β-methylaminoethoxy)-styryl]-pyridine were obtained.

1. customfreshly removed from a bomb
2. temperatureAfter cooling
3. customthe contents of the autoclave were evaporated
4. dissolutionthe residue was dissolved in dilute acetic acid
5. extractionthe solution was extracted twice with ether
6. customto remove weakly basic products
7. extractionwas extracted with ethyl acetate
8. dry with materialAfter drying the ethyl acetate
9. extractionextract with sodium sulfate
10. distillationdistilling off the solvent
11. customan oily residue was obtained which
12. customcrystallized