HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
3-Nitrophenylboronic Acid → 3-Fluoro-N-(6-methyl-3'-nitrobiphenyl-3-yl)-5-(trifluoromethyl)benzamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 3-Nitrophenylboronic Acid | HCID 1677 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 3-fluoro-N-(3-iodo-4-methylphenyl)-5-(trifluoromethyl)benzamide | HCID 69044093 | — |
| Katalysator | HCID 178418397 | HCID 178418397 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Produkt | 3-Fluoro-N-(6-methyl-3'-nitrobiphenyl-3-yl)-5-(trifluoromethyl)benzamide | HCID 69045321 | 97,8% |
Reaktionsschritte
(3-Nitrophenyl)boronic acid (1.7 g, 10.0 mmol) was mixed with 3-fluoro-N-(3-iodo-4-methylphenyl)-5-(trifluoromethyl)benzamide (4.30 g, 10.2 mmol) and potassium carbonate (2.5 g, 18 mmol) in toluene (75.00 mL), ethanol (11.00 mL) and water (10.00 mL) and was degassed. To the mixture was added tetrakis(triphenylphosphine)palladium(0) (0.50 g, 0.43 mmol) and the resulting mixture was heated to reflux for 18 hours. The reaction was extracted with ethyl acetate and the organic extracts were washed with water, saturated NaCl, dried (MgSO4) and then concentrated in vacuo. The residue was purified by column chromatography using 20% EtOAc/hexanes to give the product (4.09 g, 96% yield). MS (EI) m/z=419 (M+H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08513270B2 |
| Quelldatensatz | uspto-grants-2013_08 |
| ORD ID | ord-db1f00d1fd534239b44c5a55ef158143 |
| Quellennotiz | uspto-grants-2013_08 |