HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ethyl Acetate → Ethyl 4-(2-formylphenylthio)butyrate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ethyl Acetate | HCID 8857 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | o-Fluorobenzaldehyde | HCID 67970 | — |
| Edukt | Ethyl 4-sulfanylbutanoate | HCID 271824 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | Ethyl 4-(2-formylphenylthio)butyrate | HCID 18533389 | 67% |
Reaktionsschritte
Under an argon atmosphere, 2-fluorobenzaldehyde (5 g) was dissolved in 15 ml of dimethylformamide and potassium carbonate (8.35 g) was added. Ethyl 4-mercaptobutyrate (8.6 ml) was added at room temperature and was stirred at room temperature for 14 hours. After the addition of 100 ml of ethyl acetate, the mixture was washed with 50 ml of water twice, 50 ml of a 0.5N hydrochloric acid, and 50 ml of water three times. After drying with anhydrous sodium sulfate, the mixture was concentrated. The concentrated matter was subjected to silica gel chromatography (hexane/ethyl acetate=4/1) purification. The resulting effective fractions were concentrated to yield ethyl 4-(2-formylphenylthio)butyrate (6.86 g, Yield 67%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06566535B1 |
| Quelldatensatz | uspto-grants-2003_05 |
| ORD ID | ord-be89ac69ae664e8a997bd87039fc1230 |
| Quellennotiz | uspto-grants-2003_05 |