反应详情

In 50 ml of anhydrous THF was suspended 4.9 g of lithium aluminum hydride, and a solution of 3 g of 6-benzyl -5,7-dioxo-octahydropyrrolo[3.4-b]pyridine in 50 ml of anhydrous THF was added thereto dropwise with stirring while cooling with ice. After the addition, the reaction mixture was heated under reflux for 6 hours. After completion of the reaction, 4.9 ml of water, 4.9 ml of aqueous ammonia, and 15 ml of water were added to the reaction mixture in this order while cooling with ice, followed by stirring for 30 minutes. The reaction mixture was filtered through Celite®, and the filter cake was washed with THF (100 ml×4). The combined filtrate and washings were dried over anhydrous sodium sulfate and concentrated to yield 2.49 g of the titled compound as an oily substance.

1. temperaturewhile cooling with ice
2. additionAfter the addition
3. temperaturethe reaction mixture was heated
4. temperatureunder reflux for 6 hours
5. additionwere added to the reaction mixture in this order
6. temperaturewhile cooling with ice
7. stirringby stirring for 30 minutes
8. filtrationThe reaction mixture was filtered through Celite®
9. washthe filter cake was washed with THF (100 ml×4)
10. dry with materialThe combined filtrate and washings were dried over anhydrous sodium sulfate
11. concentrationconcentrated