反应详情

In a 500 ml three-necked flask, 41.08 g (0.2 mol) of 3-{3-([1,3]dioxolan-2-yl)propylamino}-1-aminobutane are added to 65 g of 33% strength hydrochloric acid and 100 ml of water and the mixture is stirred vigorously for three hours. It is then neutralized by dropwise addition of 100 ml of 30% strength sodium hydroxide solution, and the neutralized solution is subjected to extraction with CH2Cl2. The organic extracts are dried over sodium carbonate and concentrated. This gives 27.54 g of a reddish liquid. Distillation under a high vacuum (overhead temperature=34° C., p=0.006 mbar) gives 15.87 g of 1,5-diazabicyclo[4.3.0]nonane as a colourless oil.

1. extractionthe neutralized solution is subjected to extraction with CH2Cl2
2. dry with materialThe organic extracts are dried over sodium carbonate
3. concentrationconcentrated
4. distillationDistillation under a high vacuum (overhead temperature=34° C., p=0.006 mbar)