反应详情

2N Hydrochloric acid was added to a solution of 1.10 g of homopiperazine in 15 ml of water at room temperature until a pH of 2 was attained. Then, 40% aqueous sodium acetate and 1.28 g of ethyl chloroformate were added alternately in portions within the pH range of 2.0 to 3.5, and the resultant mixture was stirred at room temperature for 2 hours. The reaction mixture was washed with ethyl acetate, and the aqueous layer was saturated with potassium carbonate and extracted with ethyl acetate. The organic layer was washed with saturated aqueous solution of sodium chloride, dried over anhydrous sodium sulfate and concentrated under reduced pressure to give 1.27 g of ethyl 1-homopiperazinecarboxylate.

1. washThe reaction mixture was washed with ethyl acetate
2. extractionextracted with ethyl acetate
3. washThe organic layer was washed with saturated aqueous solution of sodium chloride
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationconcentrated under reduced pressure