反应详情

Methanesulfonyl chloride (18.9 g, 0.1655 mol) was added dropwise at 0° C. to a solution of N-benzyl ethanolamine (10 g, 0.0662 mol, from step (i) above) and triethylamine (27.6 ml, 0.1987 mol) in dichloromethane (100 ml). The reaction mixture was stirred at RT for 3 h under nitrogen atmosphere and partitioned between water and dichloromethane. The organic layer was separated, washed with water and brine and dried over sodium sulfate. Thes solvent was evaporated under reduced pressure and the residue was purified by column chromatography over silica gel using 3% methanol in dichloromethane, as eluent to give the sub-title compound (12 g) as a solid.

1. custompartitioned between water and dichloromethane
2. customThe organic layer was separated
3. washwashed with water and brine
4. dry with materialdried over sodium sulfate
5. customThes solvent was evaporated under reduced pressure
6. customthe residue was purified by column chromatography over silica gel using 3% methanol in dichloromethane, as eluent