HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
2,3,5-Trifluorobenzaldehyde → 2-(4-Tert-butylpiperazin-1-yl)-3,5-difluorobenzaldehyde
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 2,3,5-Trifluorobenzaldehyde | HCID 2776950 | — |
| Edukt | 1-Tert-butylpiperazine | HCID 3530572 | — |
| Edukt | Water ethylacetate | HCID 22728543 | — |
| Lösungsmittel | 1,4-Dioxane | HCID 31275 | — |
| Produkt | 2-(4-Tert-butylpiperazin-1-yl)-3,5-difluorobenzaldehyde | HCID 57774386 | 21% |
Reaktionsbedingungen
| Temperatur | 80 °C |
|---|
Reaktionsschritte
1-tert-Butylpiperazine (2.3 g, 16.2 mmol) and 2,3,5-trifluorobenzaldehyde (2.6 g, 16.2 mmol) were combined in dioxane and heated to 80° C. overnight. The yellow suspension was poured into H2O/ethyl acetate and the organic layer extracted with 1N HCl. The acidic extract was neutralized with 6N NaOH and extracted with ethyl acetate to yield the crude product as a yellow solid. This solid was purified by silica column to give 2-(4-tert-butylpiperazin-1-yl)-3,5-difluorobenzaldehyde as a yellow solid (0.96 g., 3.4 mmol, 21% yield) 1H-NMR (300 MHz, CDCl3) δ 10.52, (1H, s); 7.35 (1H, m); 7.07 (1H, m); 3.22 (4H, m); 2.71 (4H, m); 1.12 (9H, s) ppm.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08163737B2 |
| Quelldatensatz | uspto-grants-2012_04 |
| ORD ID | ord-e47b4d1178c74676b5fc884f3b91b4aa |
| Quellennotiz | uspto-grants-2012_04 |