Sodium Hydroxide → HCID 23077364, compound

In ethanol (10 ml) was dissolved 0.60 g (2 mmol) of ethyl 2-(benzyloxycarbonylamino)-2-methylpropane-1-sulfinate, and 0.9 g (2.2 mmol) of 10% aqueous sodium hydroxide solution was slowly dropped thereinto under ice-cooling. The reaction was carried out at room temperature for 1 hour and then the ethanol was distilled off. Water (10 ml), 0.18 g (2.2 mmol) of sodium acetate and 0.25 g (2.2 mmol) of hydroxylamine-O-sulfonic acid were added to the residue, and the reaction was carried out at room temperature for 1 hour. The reaction mixture was poured into water, followed by three runs of extraction with ethyl acetate. The extract solution was washed with saturated aqueous sodium hydrogencarbonate solution and then saturated aqueous sodium chloride solution, and dried over anhydrous sodium sulfate. The solvent was distilled off and 0.49 g (yield 86%) of the thus obtained crude 2-(benzyloxycarbonylamino)-2-methylpropane-1-sulfonamide was used without further purification in the subsequent reaction.

1. additionwas slowly dropped
2. temperatureunder ice-cooling
3. distillationthe ethanol was distilled off
4. waitthe reaction was carried out at room temperature for 1 hour
5. extractionfollowed by three runs of extraction with ethyl acetate
6. washThe extract solution was washed with saturated aqueous sodium hydrogencarbonate solution
7. dry with materialsaturated aqueous sodium chloride solution, and dried over anhydrous sodium sulfate
8. distillationThe solvent was distilled off

ORD record

ord-229c222719b84799beed032c43d604bb

Source dataset

uspto-grants-2007_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07161032B2