HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
1,4-Diazabicyclo(3.2.2)nonan-3-one → 1,4-Diazabicyclo(3.2.2)nonane
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 1,4-Diazabicyclo(3.2.2)nonan-3-one | HCID 4401850 | — |
| Edukt | Aluminium lithium hydride | HCID 21226445 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | 1,4-Diazabicyclo(3.2.2)nonane | HCID 398407 | 64,5% |
Reaktionsschritte
Lithium aluminum hydride (2.0 g, 51.4 mmoles) was slurried in 250 ml of dry tetrahydrofuran and 3-oxo-1,4-diazabicyclo[3.2.2]nonane (3.6 g, 25.7 mmoles) was added carefully as a solid in one portion at room temperature. The resulting mixture was then heated to a gentle reflux for 20 hours. The reaction was cooled to room tempeature and quenched by slow addition of 2.5 ml water. The salts were filtered and washed several times with diethyl ether totaling 1.0 1. These washings and the supernatant were combined, dried over magnesium sulfate and concentrated to give 2.09 g (64.5%) of the title compound as a pale yellow oil.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04775668 |
| Quelldatensatz | uspto-grants-1988_10 |
| ORD ID | ord-c29499e62b974f038a1fcb19a31047d6 |
| Quellennotiz | uspto-grants-1988_10 |