反应详情

温度

65 °C

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 roomtemperature for two days. The solvent was evaporated and the residue was dissolved in CH2Cl2. The organic layer was washed twice with 0.3 M 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. customThe solvent was evaporated
2. dissolutionthe residue was dissolved in CH2Cl2
3. washThe organic layer was washed twice with 0.3 M KHSO4 and once with brine
4. dry with materialThe combined organic layer was dried (Na2SO4)
5. filtrationfiltered
6. customevaporated
7. customThe crude product was purified by flash chromatography