HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Methanol → 4-[4-[4-(4-Pyridyl)piperazin-1-yl]phenoxy]butyric acid, hydrochloride salt
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Methanol | HCID 887 | — |
| Edukt | Pyridinium chloride | HCID 10176127 | — |
| Edukt | 4-[4-[4-(4-Pyridyl)piperazin-1-yl]phenoxy]butyric acid | HCID 18918511 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | 4-[4-[4-(4-Pyridyl)piperazin-1-yl]phenoxy]butyric acid, hydrochloride salt | HCID 131719612 | 81,3% |
Reaktionsschritte
A mixture of the product from Example 26 (1.5 g) and methanol (80 ml) was heated to reflux with stirring, and solid pyridine hydrochloride (0.5 g) was added. Heating was stopped and ethyl acetate (10 ml) was added. The reaction mixture was evaporated until a slight turbidity was observed. On further cooling, a precipitate formed which was collected, washed with ethyl acetate and dried to give the title compound (1.33 g) as a beige solid: m.p.>240° C. (dec); NMR (d6 -DMSO) δ 1.90 (2H, m), 2.36 (2H, t), 3.17 (4H, m), 3.83 (4H, m), 3.91 (2H, t), 6.89 (4H, q), 7.26 (2H, d), 8.25 (2H, d), 12.1 (1H, br), 13.75 (1H, br); m/Z 342 (M+H)+ ; calculated for C19H23N3O3. 1.0 HCl: C, 60.4%; H, 6.4%; N, 11.1%; found: C, 60.0%; H, 6.4%, N, 10.8%.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05728701 |
| Quelldatensatz | uspto-grants-1998_03 |
| ORD ID | ord-49e1ae57538b4195be3dcdaff27940ff |
| Quellennotiz | uspto-grants-1998_03 |