反应详情

温度

0 °C

A mixture of 2-tert-butoxycarbonylaminoethanol (32.7 g, 203 mmol), triethylamine (34 ml), p-toluenesulfonyl chloride (38.7 g, 203 mmol), 4-dimethylaminopyridine (0.10 g) and dichloromethane (500 ml) was stirred at 0° C. for 4 hours. The reaction mixture was washed successively with water, 1N hydrochloric acid, a saturated aqueous sodium hydrogencarbonate solution and a saturated aqueous sodium chloride solution. The organic layer was dried over anhydrous magnesium sulfate and the solvent was distilled off under reduced pressure. The resulting residue was purified by a silica gel column chromatography (eluent:ethyl acetate/n-hexane= 1/5) to obtain 48.2 g of 2-tert-butoxycarbonylaminoethyl 4-toluenesulfonate.

1. washThe reaction mixture was washed successively with water, 1N hydrochloric acid
2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
3. distillationthe solvent was distilled off under reduced pressure
4. customThe resulting residue was purified by a silica gel column chromatography (eluent:ethyl acetate/n-hexane= 1/5)