反应详情

A solution of tert-butyl 4-(1-bromo-2-oxoethyl)-1-piperidinecarboxylate (21 g) and N,N′-dimethylthiourea (6.0 g) in ethanol (300 ml) was heated under reflux. The reaction mixture was concentrated under reduced pressure, the residue was dissolved in ethyl acetate and water, and the aqueous layer was collected by separation. The residue was basified with an aqueous potassium carbonate solution and extracted with chloroform. The extract was dried over anhydrous sodium sulfate and the solvent was distilled off under reduced pressure to obtain the title compound as a pale yellow solid (12 g, 57%).

1. temperatureunder reflux
2. concentrationThe reaction mixture was concentrated under reduced pressure
3. dissolutionthe residue was dissolved in ethyl acetate
4. customwater, and the aqueous layer was collected by separation
5. extractionextracted with chloroform
6. dry with materialThe extract was dried over anhydrous sodium sulfate
7. distillationthe solvent was distilled off under reduced pressure