HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Diethyl Oxalate → Ethyl 2,4-dioxo-4-(2,4,6-trimethylphenyl)butanoate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Diethyl Oxalate | HCID 7268 | — |
| Edukt | Ethanone, 1-(2,4,6-trimethylphenyl)- | HCID 15461 | — |
| Edukt | Sodium hydride | HCID 24758 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Produkt | Ethyl 2,4-dioxo-4-(2,4,6-trimethylphenyl)butanoate | HCID 14945000 | 66,7% |
Reaktionsschritte
To a solution of 2', 4', 6'-trimethylacetophenone (15 g, 92.6 mmol) and diethyl oxalate (20 g, 139 mmol) in 500 mL of anhydrous toluene was cautiously added 7.4 g of NaH (60% dispersion in mineral oil). The reaction mixture was slowly heated to reflux under N2. It was refluxed for about 20 minutes, then cooled, poured into ice-cold aqueous HCl solution, and extracted with ether. The extracts were washed with brine, dried over Na2SO4, filtered through a short silica gel pad and concentrated to give 16.2 g of a red oil which was used in the next reaction without further purification.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05723608 |
| Quelldatensatz | uspto-grants-1998_03 |
| ORD ID | ord-54fc6a8a376c4fd9a41d798a9116e90e |
| Quellennotiz | uspto-grants-1998_03 |