反应详情

To a suspension of glycine ethyl ester hydrochloride (9.45 g) in methylene chloride (100 ml) were added triethylamine (18.9 ml) and 2-nitrobenzenesulfonyl chloride (10.0 g) in succession under cooling with ice and the mixture was stirred at room temperature for 2 days. To the reaction mixture was added 1N hydrochloric acid under cooling with ice, followed by extraction with methylene chloride. The organic layer was washed with saturated aqueous solution of sodium hydrogencarbonate, then saturated sodium chloride solution, and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure and the precipitated crystals were washed with a mixed solvent of n-hexane and diethyl ether, collected by filtration and air-dried to obtain the title compound (10.8 g).

1. temperatureunder cooling with ice
2. temperatureunder cooling with ice
3. extractionfollowed by extraction with methylene chloride
4. washThe organic layer was washed with saturated aqueous solution of sodium hydrogencarbonate
5. dry with materialsaturated sodium chloride solution, and dried over anhydrous sodium sulfate
6. distillationThe solvent was distilled off under reduced pressure
7. washthe precipitated crystals were washed with a mixed solvent of n-hexane and diethyl ether
8. filtrationcollected by filtration
9. customair-dried