反应详情

温度

25 °C

A mixture of tert-butyl 2,4-dioxo-1,3,8-triaza-8-spiro[4.5]decane-carboxylate (4.9 g, 18.2 mmol), dimethylsulfate (2.9 g, 23 mmol), potassium carbonate (10.8 g, 78.3 mmol) and DMF (60 mL) was stirred approximately 60 hours at 25° C. The mixture was concentrated and the residue was partitioned between ethyl acetate and water. The ethyl acetate layer was separated, washed with water (3×), dried (Na2SO4), filtered and concentrated to give tert-butyl 2,4-dioxo-3-methyl-1,3,8-triaza-8-spiro[4.5]decanecarboxylate (4.7 g, 16.6 mmol), m.p. 206°-208° C.

1. concentrationThe mixture was concentrated
2. customthe residue was partitioned between ethyl acetate and water
3. customThe ethyl acetate layer was separated
4. washwashed with water (3×)
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated