HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
2-(Methylamino)ethanol → 1-{6-[(2-Hydroxyethyl)(methyl)amino]naphthalen-2-yl}ethan-1-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 2-(Methylamino)ethanol | HCID 8016 | — |
| Edukt | 1-(6-Hydroxy-2-naphthyl)ethan-1-one | HCID 82631 | — |
| Edukt | Sodium Bisulfite | HCID 23665763 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | 1-{6-[(2-Hydroxyethyl)(methyl)amino]naphthalen-2-yl}ethan-1-one | HCID 18761121 | 73% |
Reaktionsschritte
A mixture of 4.15 g (55.5 mmol) NaHSO3, 8 mL of water, 0.78 g (4.19 mmol) of 1-(6-hydroxy-2-naphthyl)-1-ethanone (prepared as described in Example 1(b)), and 8 mL of 2-methylaminoethanol was heated and stirred in a steel bomb at 140° C. for 28 hours. After cooling, the mixture was distributed between ethyl acetate and water (500 mL and 200 mL, respectively). The organic layer was dried and evaporated to leave raw 1-(6-(2-hydroxyethyl-methylamino)-2-naphthyl)-1-ethanone (0.749 g, 73%) of which was further purified by radial chromatography (4 mm SiO3, CH2Cl2).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06274119B1 |
| Quelldatensatz | uspto-grants-2001_08 |
| ORD ID | ord-3f12de9b3cec48ca8929e082b8c70a1c |
| Quellennotiz | uspto-grants-2001_08 |