反应详情

温度

100 °C

The suspension of ethyl N-benzyl-3-oxo-4-piperidine-carboxylate hydrochloride (8.9 g, 30 mmol) and thiourea (4.56 g, 60 mmol) in the solution of sodium methoxide in methanol (34 mL, 25% wt) was stirred at 100° C. in a sealed tube overnight. Iodomethane (5.1 g, 42 mmol) was added dropwise to the reaction mixture after cooled to room temperature and stirred at room temperature for 1 hr. Solvent was removed in vacuo and residue was dissolved in water (100 mL) and was extracted by CHCl3 and i-PrOH (3:1, 10×40 mL), dried over sodium sulfate. Solvent was removed in vacuo, product was obtained as a beige powder (7.6 g, 88%).

1. temperatureafter cooled to room temperature
2. stirringstirred at room temperature for 1 hr
3. customSolvent was removed in vacuo and residue
4. dissolutionwas dissolved in water (100 mL)
5. extractionwas extracted by CHCl3 and i-PrOH (3:1, 10×40 mL)
6. dry with materialdried over sodium sulfate
7. customSolvent was removed in vacuo