反应详情

温度

65 °C

A suspension of 1,4-dioxa-spiro[4.5]decan-8-one (10.0 g, 64.0 mmol) in 64 mL of methanol was treated with a solution of ammonium carbonate (18.4 g, 192 mmol) in 64 mL of water. Potassium cyanide (6.14 g, 96.0 mmol) was added and the mixture was stirred at 65° C. for 18 h. It was cooled to room temperature and a precipitate was formed. The precipitate was collected by filtration to give a white solid and the filtrate was extracted with ethyl acetate. The portion of ethyl acetate was concentrated to afford also a white solid. Both solids were combined to afford 9,12-dioxa-1,3-diaza-dispiro[4.2.4.2]tetradecane-2,4-dione (9.80 g, 68%)

1. temperatureIt was cooled to room temperature
2. customa precipitate was formed
3. filtrationThe precipitate was collected by filtration
4. customto give a white solid
5. extractionthe filtrate was extracted with ethyl acetate
6. concentrationThe portion of ethyl acetate was concentrated
7. customto afford also a white solid