HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → Diethyl 2-(4-methoxyphenyl)malonate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Diethyl Carbonate | HCID 7766 | — |
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | Ethyl 4-methoxyphenylacetate | HCID 84174 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | Diethyl 2-(4-methoxyphenyl)malonate | HCID 2785178 | — |
Reaktionsschritte
27.7 g of ethyl 4-methoxyphenylacetate and 34 ml of diethyl carbonate were dissolved in 150 ml of N,N-dimethylformamide, and the solution was subjected to reflux under heating, while gradually adding 6.5 g of sodium hydride for 1 hour. After further refluxing under heating for 2 hours, the resulting reaction solution was poured into a mixture of ice water and hydrochloric acid, followed by extraction with ethyl acetate. The resulting organic layer was washed with water, and then dried to distill off the solvent. The residue thus obtained was purified by silica gel column chromatography using toluene as an eluant, thereby obtaining 26.7 g of ethyl 2-ethoxycarbonyl-2-(4-methoxyphenyl)acetate in the form of light yellow oil.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05620991 |
| Quelldatensatz | uspto-grants-1997_04 |
| ORD ID | ord-cdb199cccde4424c84d1054619df02b1 |
| Quellennotiz | uspto-grants-1997_04 |