反应详情

A suspension of 9,12-dioxa-1,3-diazadispiro[4.2.4.2]tetradecane-2,4-dione (6.33 g, 28.0 mmol) in HCl (6N) (28 mL, 168 mmol) and EtOH (66.0 mL) was stirred at RT for 18 hours. The mixture was partially evaporated (about ½ volume), cooled in an ice bath and brought to a pH of approximately 10. The aqueous layer was extracted with DCM (2×200 mL), and the aqueous layer concentrated. The residue was triturated with THF (2×100 mL), and solids were removed by filtration. The filtrate was evaporated to afford the title compound as a white solid.

1. customThe mixture was partially evaporated (about ½ volume)
2. temperaturecooled in an ice bath
3. extractionThe aqueous layer was extracted with DCM (2×200 mL)
4. concentrationthe aqueous layer concentrated
5. customThe residue was triturated with THF (2×100 mL), and solids
6. customwere removed by filtration
7. customThe filtrate was evaporated