反応 #632019

反応方程式

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

dioxane

→

1,4-diazabicyclo[3.2.2]nonane

収率 78.0%

溶媒

water

反応条件

後処理

1. 1
   温度The mixture was refluxed for 6 h
2. 2
   その他to reach room temperature
3. 3
   ろ過filtered off via glass
4. 4
   ろ過filter
5. 5
   その他The solvent was evaporated
6. 6
   workup.DISTILLATIONthe residue was distilled
7. 7
   その他at 90° C.

実験手順

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.

出典