HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Cyclopropylamine → HCID 57687389, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Cyclopropylamine | HCID 69828 | — |
| Edukt | 2,4,6-Trifluorobenzoic acid | HCID 520373 | — |
| Lösungsmittel | Pyridine | HCID 1049 | — |
| Produkt | HCID 57687389 | HCID 57687389 | 70,2% |
Reaktionsschritte
2,4,6-Trifluorobenzoic acid (9.0 g, 34.1 mmol) and cyclopropylamine (14.65 g, 256 mmol) were stirred in pyridine (300 mL) at 120° C. in a sealed tube for 22 h. The solution was concentrated in vacuo. The residue was taken up in water (30 mL) and the solution was acidified to pH 2-3 with 1N HCl. The resulting precipitate was collected by filtration to yield 5.1 g (47%) of clean desired product as a beige solid. 1H NMR (400 MHz, DMSO-d6): δ 8.05 (s, 1H), 6.65 (d, 1H, J=8.0 Hz), 6.42 (t, 1H, J=10.8 Hz), 2.42-2.48 (m, 1H), 0.76-0.83 (m, 2H), 0.45-0.51 (m, 2H). MS (ES) [m+H] calc'd for C10H9F2NO2, 213; found 213.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08063066B2 |
| Quelldatensatz | uspto-grants-2011_11 |
| ORD ID | ord-e87a64e4ef554c93bbfde3a7d51289c7 |
| Quellennotiz | uspto-grants-2011_11 |