HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ethylene Glycol → Methyl 1,4-dioxaspiro[4.5]decane-7-carboxylate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ethylene Glycol | HCID 174 | — |
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) | HCID 466102 | — |
| Edukt | Methyl 3-oxocyclohexane-1-carboxylate | HCID 566099 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Produkt | Methyl 1,4-dioxaspiro[4.5]decane-7-carboxylate | HCID 372311 | — |
Reaktionsschritte
Methyl 3-oxocyclohexanecarboxylate (930 mg) and pyridinium p-toluenesulfonate (299 mg) were combined in toluene (29.8 mL) to give a colorless solution. Ethylene glycol (0.996 mL) was added and the reaction was refluxed under Dean-Stark conditions for 2 days. The reaction was cooled to room temperature, triethylamine was added, and then the mixture was concentrated by rotary evaporation. The residue was purified by regular phase flash column chromatography (Analogix 0-40% hexane/ethyl acetate).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09034875B2 |
| Quelldatensatz | uspto-grants-2015_05 |
| ORD ID | ord-89ae61a478bb4ddc8bfe5bc0a9a34275 |
| Quellennotiz | uspto-grants-2015_05 |