Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hydroxyamine hydrochloride | HCID 443297 | — |
| Edukt | 1-Benzylpiperidine-4-acetonitrile | HCID 562499 | — |
| Edukt | Sodium | HCID 5360545 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | HCID 178510845 | HCID 178510845 | — |
Reaktionsschritte
Sodium metal (0.8 g, 34.78 mmol) was dissolved in dry methanol (10 mL) at 0-10° C. and this solution was added slowly into a suspension of hydroxylamine hydrochloride (2.43 g, 34.96 mmol) in methanol (10 mL) at room temperature. The reaction mixture was stirred for 10 min until a clear solution was obtained, 2-(1-Benzylpiperidin-4-yl)acetonitrile (compound of Example 27; 3 g, 13.99 mmol) in dry methanol (20 mL) was added into the resulting reaction mixture and heated at 75° C. for 13 h. The solvent was evaporated at 50° C. to 55° C. and the crude product obtained was purified by column chromatography (silica gel, chloroform-methanol) to afford the title compound.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US08629277B2 |
|---|
| Quelldatensatz | uspto-grants-2014_01 |
|---|
| ORD ID | ord-798425f4702045289f068de3a3155a8c |
|---|
| Quellennotiz | uspto-grants-2014_01 |
|---|