反应详情

温度

68 °C

A mixture of tert-butyl 3-((4-oxo-1-phenyl-1,3,8-triazaspiro[4.5]decan-3-yl)methyl)benzoate (300 mg, 0.71 mmol, 1 equiv), 4-iodo-1-(4-methoxyphenyl)butan-1-one (216.5 mg, 0.71 mmol, 1 equiv), and potassium carbonate (285.2 mg, 2.136 mmol, 3 equiv) in N,N-dimethylformamide was stirred at 68° C. for 16 h. After cooling the reaction mixture, the crude mixture was partitioned between ethyl acetate and water. The organic layer was dried over MgSO4, filtered, concentrated, and the crude residue was purified using the Biotage flash chromatography system (SNAP 10 g cartridge, Rf=0.4, gradient—1%-8% methanol in dichloromethane) to afford the title compound as an oil (100 mg, 25%); MS for C36H43N3O5 m/z 598.3 (M+H)+.

1. temperatureAfter cooling the reaction mixture
2. customthe crude mixture was partitioned between ethyl acetate and water
3. dry with materialThe organic layer was dried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated
6. customthe crude residue was purified