Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Ethanol | HCID 702 | — |
| Edukt | Water | HCID 962 | — |
| Edukt | 1-Benzyl-4-(4-nitrophenyl)piperazine | HCID 2747427 | — |
| Katalysator | Iron | HCID 23925 | — |
| Lösungsmittel | Acetic Acid | HCID 176 | — |
| Produkt | 4-(4-Benzylpiperazin-1-yl)aniline | HCID 737259 | — |
Reaktionsschritte
Iron powder (5.4 g, 97 mmol, 4 equiv) is added portionwise to an 80° C. mixture of 1-benzyl-4-(4-nitro-phenyl)-piperazine (7.2 g, 24.2 mmol), EtOH (150 mL), H2O (40 mL), and AcOH (20 mL). The reaction mixture is stirred for 1.75 h at 80° C., allowed to cool to RT, and concentrated. The residue is diluted with EtOAc and an aqueous saturated solution of Na2CO3. The layers are separated and the aqueous phase is extracted with EtOAc. The combined organic phase is washed with brine, dried (Na2SO4), filtered and concentrated to afford the title compound: ES-MS: 268.3 [MH]+; single peak at tR=1.30 min (system 1).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US08759517B2 |
|---|
| Quelldatensatz | uspto-grants-2014_06 |
|---|
| ORD ID | ord-9ac1155e7ef04fc7ab35e1595741496c |
|---|
| Quellennotiz | uspto-grants-2014_06 |
|---|