反应详情

A solution of 2-chloroethyl N-(4-octylphenyl)sulfamoylcarbamate (156 mg, 0.4 mmol) in CH3CN (10 mL) was treated with Et3N (0.14 mL, 1 mmol) and refluxed for 25 min. and cooled. A solution of 2-(3-amino-1-methylpiperidin-3-yl)acetate (62 mg, 0.33 mmol) was added and the resulting mixture was refluxed for 4 h. After removal of the solvent in vacuo, the residue was dissolved in dichloromethane (40 mL) and washed with sat. NaHCO3 (10 mL), H2O (10 mL), brine (10 mL) and dried (Na2SO4). After evaporation, the residue was purified by flash chromatography (EtOAc/hex 1:4 to EtOAc) to give the title compound (41 mg, 27%) as colorless oil. MS ESI 454.3[M+H]+, calcd for [C23H39N3O4S+H]+ 454.27.

1. temperaturerefluxed for 25 min.
2. temperaturecooled
3. temperaturethe resulting mixture was refluxed for 4 h
4. customAfter removal of the solvent in vacuo
5. dissolutionthe residue was dissolved in dichloromethane (40 mL)
6. washwashed with sat. NaHCO3 (10 mL), H2O (10 mL), brine (10 mL)
7. dry with materialdried (Na2SO4)
8. customAfter evaporation
9. customthe residue was purified by flash chromatography (EtOAc/hex 1:4 to EtOAc)