反应 #632019

反应方程式

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

dioxane

→

1,4-diazabicyclo[3.2.2]nonane

收率 78.0%

溶剂

water

反应条件

后处理

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

实验过程

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.

来源