反应详情

温度

80 °C

To a cooled to 0° C. solution of 2-benzyl-2-azaspiro[4.4]nonane-1,4-dione (20.00 g, 82.2 mmol) in THF (150 mL) was added LiAlH4 (20.93 g, 550.8 mmol) portionwise. After addition, the reaction mixture was stirred at 80° C. overnight, cooled down to rt and quenched carefully with sequential addition of EtOAc (200 mL), 15% KOH aqueous solution (40 mL) and water (100 mL). After addition, the resulting mixture was stirred at rt for 3 h, and filtered through a Celite pad, then washed with EtOAc (1 L). The filtrate was concentrated in vacuo to give the product as yellow oil (19.02 g, 100%).

1. additionAfter addition
2. temperaturecooled down to rt
3. customquenched carefully with sequential addition of EtOAc (200 mL), 15% KOH aqueous solution (40 mL) and water (100 mL)
4. additionAfter addition
5. stirringthe resulting mixture was stirred at rt for 3 h
6. filtrationfiltered through a Celite pad
7. washwashed with EtOAc (1 L)
8. concentrationThe filtrate was concentrated in vacuo