HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → N-(2-Fluoro-1,1-dimethylethyl)-2,4-difluorobenzamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | 2,4-Difluorobenzoic acid | HCID 74102 | — |
| Edukt | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Edukt | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| Edukt | 1-Fluoro-2-methylpropan-2-amine hydrochloride | HCID 13935251 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | N-(2-Fluoro-1,1-dimethylethyl)-2,4-difluorobenzamide | HCID 10198515 | 44% |
Reaktionsschritte
WSC HCl (1.15 g, 6 mmol) was added to a mixture of 2,4-difluorobenzoic acid (0.95 g, 6 mmol), 2-fluoro-1,1-dimethylethylamine hydrochloride (J. Med. Chem., 34, 29-37(1991): 0.77 g, 6 mmol), HOBt (0.81 g, 6 mmol) and triethylamine (0.91 g, 9 mmol) in methylene chloride (15 ml), and stirred at room temperature for 3 hours. The reaction mixture was concentrated, diluted with ethyl acetate and washed with saturated aqueous NaHCO3, 1N hydrochloric acid, saturated aqueous NaHCO3 and brine, successively, dried over MgSO4 and concentrated under a reduced pressure. The residue was purified by silica gel chromatography (hexane/ethyl acetate=20/1) to give the title compound (0.61 g: 44%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06936736B2 |
| Quelldatensatz | uspto-grants-2005_08 |
| ORD ID | ord-4ea4f38997dd4427b20ebededd071221 |
| Quellennotiz | uspto-grants-2005_08 |