HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium Hydroxide → 1,7,10-Trioxadispiro(2.2.4^(6).2^(3))dodecane
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | 1,4-Dioxaspiro[4.5]decan-8-one | HCID 567415 | — |
| Edukt | Trimethylsulfonium methyl sulfate | HCID 2760871 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 1,7,10-Trioxadispiro(2.2.4^(6).2^(3))dodecane | HCID 12075953 | 93% |
Reaktionsschritte
12.00 g (76.83 mmol, 1.0 equiv.) of 1,4 Cyclohexanedione ethylene ketal was added to 120 ml methylene chloride along with 18.8 g (99.88 mmol, 1.3 equiv.) of trimethyl sulfonium methyl sulfate. 40 ml 50% sodium hydroxide (NaOH) was added last and the reaction was refluxed for 24 hours. The methylene chloride was removed, 200 ml ether was added and the ether layer was washed with water. The organic layer was dried with sodium sulfate and concentrated down, leaving a yellow oil, 1,7,10-trioxa-dispiro[2.2.4.2]dodecane. (12.13 g, 93% yield). No further purification was necessary.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06664258B1 |
| Quelldatensatz | uspto-grants-2003_12 |
| ORD ID | ord-74e1ae7b45ae415898970a1391756682 |
| Quellennotiz | uspto-grants-2003_12 |