反应详情

7.8 g (36.4 mmole) of 4-(N-tert-butyloxycarbonylaminomethyl) piperidine and 8.98 g (40 mmole) of N-benzyloxycarbonyl-S-methylisothiourea was mixed in 25 mL ethanol. The mixture was heated at 60°-70° C. for six hours and left at room temperature for two days. The solvent was evaporated and the residue was dissolved in CH2C2. The organic layer was washed twice with 0.3M KHSO4 and once with brine. The combined organic layer was dried (Na2SO4), filtered and evaporated. The crude product was purified by flash chromatography using a stepwise gradient of CH2Cl2 /MeOH (100/0, 97/3, 95/5, 90/10) as eluent to yield 5.22 g (37%) of the title product.

1. temperatureThe mixture was heated at 60°-70° C. for six hours
2. customThe solvent was evaporated
3. dissolutionthe residue was dissolved in CH2C2
4. washThe organic layer was washed twice with 0.3M KHSO4 and once with brine
5. dry with materialThe combined organic layer was dried (Na2SO4)
6. filtrationfiltered
7. customevaporated
8. customThe crude product was purified by flash chromatography