反应详情

To a suspension of 1,3-diazaspiro[4.5]decane-2,4,8-trione (5.00 g, 27.4 mmol) in MeOH (91 mL) was added ammonium acetate (6.35 g, 82 mmol), and the mixture was stirred at RT for 25 minutes. To the suspension was added sodium cyanoborohydride (5.17 g, 82 mmol), and the mixture was stirred at RT. After 90 minutes, the flask was cooled, and the contents were quenched by careful addition of aqueous concentrated HCl, adjusting the pH to 7 with solid NaHCO3. The mixture was filtered through a pad of Celite® brand filter aid and concentrated in vacuo. The material was used directly in the next step.

1. stirringthe mixture was stirred at RT
2. waitAfter 90 minutes
3. temperaturethe flask was cooled
4. customthe contents were quenched by careful addition of aqueous concentrated HCl
5. filtrationThe mixture was filtered through a pad of Celite® brand
6. filtrationfilter aid
7. concentrationconcentrated in vacuo