反应详情

4-Nitrophenoxy sodium dihydrate (29.39 g), 2-(diethylamino)ethylchloride hydrochloride (25.60 g), potassium carbonate (30.17 g) and water (60 ml) were added into xylene (100 ml) and the mixture was heat-refluxed for 2 hours while mixing and continuously removing water by azeotropic distillation. After reaction, insolubles were removed by filtration. Filtrate was added with ethyl acetate (100 ml) and extracted 3 times with 1N HCl (100 ml). Aqueous layer was adjusted to pH 10 with 1N sodium hydroxide and oily substance separated was extracted 3 times with ethyl acetate (100 ml). Ethyl acetate solution was dehydrated with anhydrous magnesium sulfate and concentrated to obtain N,N-diethyl-2-(4-nitrophenoxy)ethylamine (28.19 g) as color-less oily substance.

1. temperaturethe mixture was heat-refluxed for 2 hours
2. additionwhile mixing
3. distillationcontinuously removing water by azeotropic distillation
4. customAfter reaction, insolubles
5. customwere removed by filtration
6. additionFiltrate was added with ethyl acetate (100 ml)
7. extractionextracted 3 times with 1N HCl (100 ml)
8. customseparated
9. extractionwas extracted 3 times with ethyl acetate (100 ml)
10. concentrationconcentrated