HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → 3,3-Diethyl-1,5-dioxaspiro[5.5]undecan-9-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Prenderol | HCID 8284 | — |
| Edukt | 1,4-Cyclohexanedione | HCID 12511 | — |
| Katalysator | p-Toluenesulfonic acid | HCID 6101 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Produkt | 3,3-Diethyl-1,5-dioxaspiro[5.5]undecan-9-one | HCID 67697693 | 16.365,5% |
Reaktionsschritte
30 g (0.27 mmol) of cyclohexane-1,4-dione, 35.4 g (0.27 mol) of 2,2-diethylpropane-1,3-diol and 360 mg of para-toluenesulfonic acid were heated in 200 ml of toluene on a water separator. After the mixture had been cooled to room temperature and the water of reaction separated off, the organic phase was washed with a semisaturated sodium hydrogen carbonate solution and dried over magnesium sulfate. After the solvent had been evaporated, 65 g of crude product were obtained which was purified by flash chromatography (ethyl acetate/petroleum ether=1:4). The first fraction contained the 1,4-diketal which was formed as secondary product (10 g). The main fraction contained 28.5 g (47%) of a yellow oil.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05859009 |
| Quelldatensatz | uspto-grants-1999_01 |
| ORD ID | ord-0a1588cf774c4fd8a5eee7ad372743fb |
| Quellennotiz | uspto-grants-1999_01 |