反应详情

A solution of 8.1 gm (34.9 mmol) 2(S)-ethyl-4-benzyl-3,6-dioxopiperazine in 50 mL tetrahydrofuran was added dropwise via addition funnel to a solution of 75 mL (75 mMol) lithium aluminum hydride (1M in tetrahydrofuran) and the mixture was heated at reflux for 2.5 h. The reaction was then cooled in an ice bath and was treated sequentially with 3 mL deionized water, 3 mL 5N sodium hydroxide, and 9 mL deionized water. The resulting slurry was allowed to stir for 1 hour and was then filtered. The recovered salts were rinsed with 100 mL tetrahydrofuran and 100 mL dichloromethane. The filtrate was concentrated in vacuo to afford 7.03 g (99%) of the desired piperazine.

1. temperaturethe mixture was heated
2. temperatureat reflux for 2.5 h
3. temperatureThe reaction was then cooled in an ice bath
4. additionwas treated sequentially with 3 mL
5. filtrationwas then filtered
6. washThe recovered salts were rinsed with 100 mL tetrahydrofuran and 100 mL dichloromethane
7. concentrationThe filtrate was concentrated in vacuo