HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
1,3-Cyclohexanedione → 3,3-Dimethyl-1,5-dioxaspiro[5.5]undecan-8-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 1,3-Cyclohexanedione | HCID 10434 | — |
| Edukt | Neopentyl glycol | HCID 31344 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Produkt | 3,3-Dimethyl-1,5-dioxaspiro[5.5]undecan-8-one | HCID 15344749 | — |
Reaktionsschritte
125 g (630 mmole) 3,3-dimethyl-1,5-dioxa-spiro[5,5]undecan-8-one, which was obtained by the azeotropic acetylation of cyclohexane-1,3-dione with 2,2-dimethylpropane-1,3-diol in toluene as a solvent using p-toluenesulphonic acid as a catalyst, and 59 g (630 mmole) dimethylammonium methylene chloride were stirred at room temperature in 400 ml of dry acetonitrile. After adding 1 ml acetyl chloride the mixture was stirred for a further 3 hours at room temperature, whereupon a clear colourless solution was obtained. 800 ml of dry ether were then added drop-wise to the reaction mixture, whereupon the hydrochloride crystallised out. 158 g of (18) were obtained (98% theoretical).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05733936 |
| Quelldatensatz | uspto-grants-1998_03 |
| ORD ID | ord-170e488e116e4e0492b95134d1d42168 |
| Quellennotiz | uspto-grants-1998_03 |