HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sulfuric Acid → (1-Benzyl-4-(4-(pyridin-4-yl)piperazin-1-yl)piperidin-4-yl)methanamine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sulfuric Acid | HCID 1118 | — |
| Edukt | Aluminium lithium hydride | HCID 21226445 | — |
| Edukt | 1-Benzyl-4-(4-(pyridin-4-yl)piperazin-1-yl)piperidine-4-carbonitrile | HCID 68629503 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | (1-Benzyl-4-(4-(pyridin-4-yl)piperazin-1-yl)piperidin-4-yl)methanamine | HCID 57989584 | 85% |
Reaktionsschritte
H2SO4 (1.5 equiv.) was added to a suspension of LAH (3 equiv.) in THF (32 ml) at 0° C. and the mixture was stirred at room temperature for 0.5 h. A solution of 1-benzyl-4-(4-(pyridin-4-yl)piperazin-1-yl)piperidine-4-carbonitrile (5.54 mmol, 1 equiv.) in THF was added under cooled conditions and the resulting reaction mixture was heated to 50° C. for 16 h. The reaction was quenched with THF/H2O solution, filtered and the solid residue washed with excess ethyl acetate. The organic layer was given a brine wash, dried over sodium sulfate and the solvent was removed under reduced pressure. The resulting crude product was used for the next step without further purification. Yield: 85%.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08541573B2 |
| Quelldatensatz | uspto-grants-2013_09 |
| ORD ID | ord-50e858841fe74112aab7551f9fc91960 |
| Quellennotiz | uspto-grants-2013_09 |