Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 1-Chloro-2-(diethylamine)ethane hydrochloride | HCID 13363 | — |
| Edukt | HCID 178526976 | HCID 178526976 | — |
| Lösungsmittel | O-Xylene | HCID 7237 | — |
| Produkt | Diethyl[2-(4-nitrophenoxy)ethyl]amine | HCID 88294 | 79,5% |
Reaktionsschritte
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.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US06300368B1 |
|---|
| Quelldatensatz | uspto-grants-2001_10 |
|---|
| ORD ID | ord-5642302a26bc4e7a83e80cc162e8c81c |
|---|
| Quellennotiz | uspto-grants-2001_10 |
|---|