Reaktion #632019

Reaktionsgleichung

1,4-diazabicyclo[3.2.2]nonan-3-one

dioxane

→

1,4-diazabicyclo[3.2.2]nonane

Ausbeute 78.0%

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture was refluxed for 6 h
2. 2
   Sonstigeto reach room temperature
3. 3
   Filtrationfiltered off via glass
4. 4
   Filtrationfilter
5. 5
   SonstigeThe solvent was evaporated
6. 6
   workup.DISTILLATIONthe residue was distilled
7. 7
   Sonstigeat 90° C.

Vorschrift

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.

Quelle