HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Mesitylene → HCID 54300158, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Mesitylene | HCID 7947 | — |
| Edukt | Ethyl Acetate | HCID 8857 | — |
| Edukt | Benzene, 1-bromo-3,5-dichloro- | HCID 29766 | — |
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Edukt | Methyl 2-acetamido-4-methoxybenzoate | HCID 54415798 | — |
| Katalysator | Copper iodide | HCID 83717 | — |
| Produkt | HCID 54300158 | HCID 54300158 | — |
Reaktionsschritte
A mixture of 2-acetylamino-4-methoxybenzoic acid methyl ester (9.58 g, 42.92 mmol), 1-bromo-3,5-dichlorobenzene (28.80 g, 127.48 mmol), copper iodide (2.32 g, 12.18 mmol), and sodium bicarbonate (8.72 g, 103.80 mmol) in of mesitylene (60 mL) was heated to reflux. After 7 days, the mixture was allowed to cool and was diluted with ethyl acetate (300 mL). The resulting solid was removed by filtration and washed with ethyl acetate. The filtrate was concentrated in vacuo and the residue was chromatographed on silica gel eluting with hexane/ethyl acetate (9:1→1:1) to afford the product (11.6 g); m.p. 100-101° C. after trituration in hexane.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06268387B1 |
| Quelldatensatz | uspto-grants-2001_07 |
| ORD ID | ord-756f52fcbc6e470d8dd0e668fcf7c965 |
| Quellennotiz | uspto-grants-2001_07 |