Reacción #632019

Ecuación de reacción

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

dioxane

→

1,4-diazabicyclo[3.2.2]nonane

Rendimiento 78.0%

Disolventes

water

Condiciones de reacción

Tratamiento posterior

1. 1
   TemperaturaThe mixture was refluxed for 6 h
2. 2
   Otroto reach room temperature
3. 3
   Filtraciónfiltered off via glass
4. 4
   Filtraciónfilter
5. 5
   OtroThe solvent was evaporated
6. 6
   workup.DISTILLATIONthe residue was distilled
7. 7
   Otroat 90° C.

Procedimiento

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.

Fuente