HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → 3,3-Dimethyl-1,5-dioxaspiro[5.5]undecan-9-ol
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | 3,3-Dimethyl-1,5-dioxaspiro(5.5)undecan-9-one | HCID 587968 | — |
| Edukt | Aluminium lithium hydride | HCID 21226445 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | 3,3-Dimethyl-1,5-dioxaspiro[5.5]undecan-9-ol | HCID 12470096 | 91,2% |
Reaktionsschritte
To the suspension of lithium aluminum hydride (748 mg, 19.7 mmol) in tetrahydrofuran (40 ml), a tetrahydrofuran solution of 1,4-cyclohexanedione mono-2,2-dimethyltrimethylene ketal (3.9 g, 19.7 mmol) was added at 0° C. The mixture was stirred at room temperature for 3 hours. After water (0.7 ml), a 5N aqueous sodium hydroxide solution (0.7 ml), and water (2.1 ml) were sequentially added at 0° C. to the mixture, the mixture was dried over sodium sulfate, filtrated, concentrated under reduced pressure, and purified by silica gel column chromatography (elution solvent: ethyl acetate/heptane=1/2, 1/1, 2/1) to obtain the title compound (3.6 g, yield: 91.2%) as a colorless oil.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07425634B2 |
| Quelldatensatz | uspto-grants-2008_09 |
| ORD ID | ord-1ffbaa88e08e4ae99cd7446a52d0d5c7 |
| Quellennotiz | uspto-grants-2008_09 |