HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
1,4-Dioxane → 1,4-Diazabicyclo(3.2.2)nonane
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 1,4-Dioxane | HCID 31275 | — |
| Edukt | 1,4-Diazabicyclo(3.2.2)nonan-3-one | HCID 4401850 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 1,4-Diazabicyclo(3.2.2)nonane | HCID 398407 | 78% |
Reaktionsschritte
To the solution of 1,4-diazabicyclo[3.2.2]nonan-3-one (15.8 g; 113 mmol) in absolute dioxane (130 ml) LiAlH4 (4.9 g; 130 mmol) was added under argon. The mixture was refluxed for 6 h and then allowed to reach room temperature. To the reaction mixture water (5 ml in 10 ml of dioxane) was added by drops, the mixture was stirred for 0.5 hour and then filtered off via glass filter. The solvent was evaporated and the residue was distilled using Kugelrohr apparatus at 90° C. (0.1 mbar) to yield 1,4-diazabicyclo[3.2.2]nonane (11.1 g; 78%) as colourless hygroscopic material.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07915272B2 |
| Quelldatensatz | uspto-grants-2011_03 |
| ORD ID | ord-437c6a392ed34dc982d00d8ceed4ab07 |
| Quellennotiz | uspto-grants-2011_03 |