HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium Bicarbonate → 1-(2-Amino-5-chlorophenyl)-2,2,2-trifluoroethanone
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Edukt | 1-(2-Amino-5-chlorophenyl)-2,2,2-trifluoroethan-1-one--hydrogen chloride--water (1/1/1) | HCID 44181989 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Produkt | 1-(2-Amino-5-chlorophenyl)-2,2,2-trifluoroethanone | HCID 10987882 | 91% |
Reaktionsschritte
4-Chloro-2-trifluoroacetylaniline, hydrochloride hydrate (17.1 g, 62 mmol) was stirred in a mixture of toluene (100 mL) and water (50 mL). The mixture was neutralized to pH 7 with saturated NaHCO3. The organic phase was concentrated in vacuo and the residue recrystallized from heptane to give 12.5 g (91%) of the title compound as yellow needles: mp 98-99° C.; 1H NMR (300 MHz, CDCl3) δ7.70 (t, J=2 Hz, 1H), 7.32 (dd, J=2, 9 Hz, 1H), 6.7 (d, J=9 Hz, 1H), 6.44 (brs, 2H); 13C NMR (75 MHz CDCl3) δ 180.0, 151.6, 136.9, 130.1 , 120.9, 119.0, 116.8, 111.4; 19F NMR (282 MHz, CDCl3) δ-70.3.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06028237 |
| Quelldatensatz | uspto-grants-2000_02 |
| ORD ID | ord-9e66e2f6fef9454796a43c0d6ab91582 |
| Quellennotiz | uspto-grants-2000_02 |