Réaction #632019

Équation de réaction

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

dioxane

→

1,4-diazabicyclo[3.2.2]nonane

Rendement 78.0%

Solvants

water

Conditions de réaction

Traitement

1. 1
   TempératureThe mixture was refluxed for 6 h
2. 2
   Autreto reach room temperature
3. 3
   Filtrationfiltered off via glass
4. 4
   Filtrationfilter
5. 5
   AutreThe solvent was evaporated
6. 6
   workup.DISTILLATIONthe residue was distilled
7. 7
   Autreat 90° C.

Mode opératoire

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.

Source