HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triphenylphosphine → HCID 67229299, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triphenylphosphine | HCID 11776 | — |
| Edukt | HCID 53416493 | HCID 53416493 | — |
| Edukt | 2-Ethoxy-8-isothiocyanato-1,4-dihydronaphthalene | HCID 86609612 | — |
| Lösungsmittel | 1,4-Dioxane | HCID 31275 | — |
| Produkt | HCID 67229299 | HCID 67229299 | 22% |
Reaktionsschritte
A solution of the product of Example 1F (398 mg, 1.72 mmol), the product of Example 1G (473 mg, 2.07 mmol), and triphenyl phosphine (542 mg, 2.07 mmol) in dioxane (9 mL) was heated at 85° C. for 30 min. The solution was cooled to room temperature and evaporated in vacuo. The residue was chromatographed on silica gel, eluting with 25% ethyl acetate-hexane to afford the title compound as a yellow solid (150 mg, 22%). 1H NMR (DMSO-d6) δ 9.38 (s, 1H), 7.76 (m, 4H), 7.65 (d, 1H, J=8.5 Hz), 7.62 (s, 1H), 7.18 (t, 1H, J=8.2 Hz), 6.97 (d, 1H, J=8.4 Hz), 4.85 (m, 1H), 3.79 (q, 2H, J=6.7 Hz), 3.49 (m, 2H), 3.36 (m, 2H), 1.26 (t, 3H, J=6.8 Hz); MS (ESI+) m/z 401 (M+H)+.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07902236B2 |
| Quelldatensatz | uspto-grants-2011_03 |
| ORD ID | ord-b41cf446029949bbb8ffd8e5c20401fe |
| Quellennotiz | uspto-grants-2011_03 |