Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Piperazine | HCID 4837 | — |
| Edukt | 2-Ethoxy-4-fluoronitrobenzene | HCID 12918153 | — |
| Lösungsmittel | 1,4-Dioxane | HCID 31275 | — |
| Produkt | 1-(3-Ethoxy-4-nitrophenyl)piperazine | HCID 59452580 | 88,5% |
Reaktionsschritte
To 2-(ethyloxy)-4-fluoro-1-nitrobenzene (Example 116, step A) (3.0 g, 16.2 mmol) in 60 mL of dioxane was added, piperazine (4.19 g, 48.61 mmol). The mixture was heated to 120° C. 72 h. The mixture was purified by flash chromatography to give the title compound of step A (3.6 g, 14.33 mmol, 88%). 1H NMR (400 MHz, CDCl3) δ ppm 7.95 (d, J=9.34 Hz, 1H), 6.40 (dd, J=9.34, 2.56 Hz, 1H), 6.30 (d, J=2.56 Hz, 1H), 4.13 (q, J=6.96 Hz, 2H), 3.30-3.33 (m, 4H), 2.95-3.02 (m, 4H), 1.48 (t, J=6.96 Hz, 3H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08093239B2 |
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| Quelldatensatz | uspto-grants-2012_01 |
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| ORD ID | ord-2ec0442dfb1b43c096f9eb553be59801 |
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| Quellennotiz | uspto-grants-2012_01 |
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